JP6856713B2 - Laminated glass interlayer film and laminated glass manufacturing method - Google Patents

Laminated glass interlayer film and laminated glass manufacturing method Download PDF

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Publication number
JP6856713B2
JP6856713B2 JP2019137705A JP2019137705A JP6856713B2 JP 6856713 B2 JP6856713 B2 JP 6856713B2 JP 2019137705 A JP2019137705 A JP 2019137705A JP 2019137705 A JP2019137705 A JP 2019137705A JP 6856713 B2 JP6856713 B2 JP 6856713B2
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laminated glass
interlayer film
resin layer
layer
large number
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JP2020007220A (en
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紘史 北野
紘史 北野
浩彰 乾
浩彰 乾
大希 片山
大希 片山
松本 学
学 松本
中山 和彦
和彦 中山
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Sekisui Chemical Co Ltd
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Sekisui Chemical Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C27/00Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
    • C03C27/06Joining glass to glass by processes other than fusing
    • C03C27/10Joining glass to glass by processes other than fusing with the aid of adhesive specially adapted for that purpose
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
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    • B32B17/00Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B32B17/10Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
    • BPERFORMING OPERATIONS; TRANSPORTING
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    • B32B17/10Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
    • B32B17/10005Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
    • B32B17/1055Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
    • B32B17/10559Shape of the cross-section
    • B32B17/10577Surface roughness
    • B32B17/10587Surface roughness created by embossing
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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Ceramic Engineering (AREA)
  • Joining Of Glass To Other Materials (AREA)
  • Laminated Bodies (AREA)

Description

本発明は、2層以上の樹脂層が積層された合わせガラス用中間膜であって、合わせガラスの製造工程において優れた脱気性を有し、かつ、多重像の発生を防止できる合わせガラス用中間膜、及び、該合わせガラス用中間膜を含む合わせガラスに関する。 The present invention is an interlayer film for laminated glass in which two or more resin layers are laminated, which has excellent degassing properties in the manufacturing process of laminated glass and can prevent the generation of multiple images. The present invention relates to a laminated glass including a film and an interlayer film for the laminated glass.

2枚のガラス板の間に、可塑化ポリビニルブチラール等の熱可塑性樹脂を含有する合わせガラス用中間膜を挟み、互いに接着させて得られる合わせガラスは、自動車、航空機、建築物等の窓ガラスに広く使用されている。 Laminated glass obtained by sandwiching an interlayer film for laminated glass containing a thermoplastic resin such as plasticized polyvinyl butyral between two glass plates and adhering them to each other is widely used for window glass of automobiles, aircraft, buildings, etc. Has been done.

合わせガラス用中間膜は、ただ1層の樹脂層により構成されているだけではなく、2層以上の樹脂層の積層体により構成されていてもよい。2層以上の樹脂層として、第1の樹脂層と第2の樹脂層とを有し、かつ、第1の樹脂層と第2の樹脂層とが異なる性質を有することにより、1層だけでは実現が困難であった種々の性能を有する合わせガラス用中間膜を提供することができる。
例えば特許文献1には、遮音層と該遮音層を挟持する2層の保護層とからなる3層構造の合わせガラス用中間膜が開示されている。特許文献1の合わせガラス用中間膜では、可塑剤との親和性に優れるポリビニルアセタール樹脂と大量の可塑剤とを含有する遮音層を有することにより優れた遮音性を発揮する。一方、保護層は、遮音層に含まれる大量の可塑剤がブリードアウトして中間膜とガラスとの接着性が低下することを防止している。
The interlayer film for laminated glass is not only composed of only one resin layer, but may also be composed of a laminate of two or more resin layers. As the two or more resin layers, the first resin layer and the second resin layer are provided, and the first resin layer and the second resin layer have different properties, so that only one layer is sufficient. It is possible to provide an interlayer film for laminated glass having various performances that has been difficult to realize.
For example, Patent Document 1 discloses an interlayer film for laminated glass having a three-layer structure including a sound insulation layer and two protective layers sandwiching the sound insulation layer. The interlayer film for laminated glass of Patent Document 1 exhibits excellent sound insulation by having a sound insulation layer containing a polyvinyl acetal resin having excellent affinity with a plasticizer and a large amount of plasticizer. On the other hand, the protective layer prevents a large amount of plasticizer contained in the sound insulation layer from bleeding out and reducing the adhesiveness between the interlayer film and the glass.

しかしながら、このような2層以上の樹脂層が積層された合わせガラス用中間膜を用いた合わせガラスでは、合わせガラス越しに外部の光線を視認したときに、像が多重像に見えたり、光学歪みが認められたりすることがあるという問題があった。このような多重像や光学歪みの発生は、とりわけ、特許文献1に記載されたような遮音性に優れた合わせガラス用中間膜の場合に顕著に見られた。 However, in a laminated glass using such an interlayer film for laminated glass in which two or more resin layers are laminated, when an external light beam is visually recognized through the laminated glass, the image looks like a multiple image or is optically distorted. There was a problem that it was sometimes recognized. The occurrence of such multiple images and optical distortion was particularly noticeable in the case of the interlayer film for laminated glass having excellent sound insulation as described in Patent Document 1.

特開2007−331959号公報Japanese Unexamined Patent Publication No. 2007-331959

本発明者らは、2層以上の樹脂層が積層された合わせガラス用中間膜を用いた場合の多重像の発生の原因を検討した。その結果、合わせガラス用中間膜の表面に形成された凹凸に原因があることを見出した。 The present inventors have investigated the cause of the occurrence of multiple images when an interlayer film for laminated glass in which two or more resin layers are laminated is used. As a result, it was found that the cause was the unevenness formed on the surface of the interlayer film for laminated glass.

合わせガラスの製造では、通常、少なくとも2枚のガラス板の間に合わせガラス用中間膜が積層された積層体を、ニップロールを通して扱くか(扱き脱気法)、又は、ゴムバッグに入れて減圧吸引し(真空脱気法)、ガラス板と中間膜との間に残留する空気を脱気しながら圧着する。次いで、上記積層体を、例えばオートクレーブ内で加熱加圧して圧着することにより合わせガラスが製造される。合わせガラスの製造工程においては、ガラスと合わせガラス用中間膜とを積層する際の脱気性が重要である。合わせガラス用中間膜の少なくとも一方の表面には、合わせガラス製造時の脱気性を確保する目的で、微細な凹凸が形成されている。とりわけ、該凹凸における凹部を、底部が連続した溝形状(以下、「刻線状」ともいう。)を有し、隣接する該刻線状の凹部が平行して規則的に形成される構造とすることにより、極めて優れた脱気性を発揮することができる。 In the production of laminated glass, usually, a laminated body in which an interlayer film for laminated glass is laminated between at least two glass plates is handled through a nip roll (handling degassing method) or put in a rubber bag and sucked under reduced pressure. (Vacuum degassing method), the air remaining between the glass plate and the interlayer film is degassed and crimped. Next, the laminated glass is produced by heating and pressurizing the laminated body in an autoclave, for example, and crimping the laminated glass. In the manufacturing process of laminated glass, degassing property when laminating the glass and the interlayer film for laminated glass is important. Fine irregularities are formed on at least one surface of the interlayer film for laminated glass for the purpose of ensuring deaeration during the production of laminated glass. In particular, the concave portion in the unevenness has a groove shape in which the bottom is continuous (hereinafter, also referred to as "engraved line shape"), and the adjacent engraved linear concave portion is regularly formed in parallel. By doing so, extremely excellent degassing property can be exhibited.

合わせガラス用中間膜の表面に形成された凹凸は、通常は合わせガラス製造工程における圧着の際に潰されることから、得られた合わせガラスにおいてはほとんど問題になることはなかった。
しかしながら本発明者らは、2層以上の樹脂層が積層された合わせガラス用中間膜の場合には、合わせガラス製造工程を経て得られた合わせガラスにおいて、凹凸の影響が残存し、多重像の発生の原因になっていたことを見出した。
Since the unevenness formed on the surface of the interlayer film for laminated glass is usually crushed during crimping in the laminated glass manufacturing process, there is almost no problem in the obtained laminated glass.
However, in the case of an interlayer film for laminated glass in which two or more resin layers are laminated, the present inventors have the effect of unevenness remaining in the laminated glass obtained through the laminated glass manufacturing process, resulting in multiple images. I found that it was the cause of the outbreak.

即ち、2層以上の樹脂層が積層された合わせガラス用中間膜の表面にエンボスロール等を用いて凹凸を形成した場合、中間膜の表面にのみ凹凸が形成されるのみならず、加工時の圧力によって樹脂層の層間の界面にまで凹凸が転写され、界面が平滑ではなくなってしまうと考えられる。特に表面に刻線状の凹部を形成すると、該刻線状の凹部が層間の界面にも強く転写されると考えられる。合わせガラス製造工程における圧着の際に中間膜の表面の凹凸は潰されるものの、層間の界面に転写された凹凸は残存することから、該層間界面に形成された凹凸により光干渉現象が発生することが多重像の発生する原因となっていると考えられる。とりわけ、特許文献1に記載されたような遮音性に優れた合わせガラス用中間膜では、硬い保護層の表面に凹凸を形成したときに、該保護層と柔らかい遮音層との層間に凹凸が転写されやすいことから、特に多重像が発生すると考えられる。 That is, when unevenness is formed on the surface of the interlayer film for laminated glass in which two or more resin layers are laminated by using embossing roll or the like, not only the unevenness is formed only on the surface of the interlayer film, but also during processing. It is considered that the pressure transfers the unevenness to the interface between the layers of the resin layer, and the interface becomes not smooth. In particular, when a carved line-shaped recess is formed on the surface, it is considered that the carved line-shaped recess is strongly transferred to the interface between the layers. Although the unevenness on the surface of the interlayer film is crushed during crimping in the laminated glass manufacturing process, the unevenness transferred to the interface between the layers remains, so that the unevenness formed at the interface between the layers causes a light interference phenomenon. Is considered to be the cause of the occurrence of multiple images. In particular, in the interlayer film for laminated glass having excellent sound insulation as described in Patent Document 1, when unevenness is formed on the surface of the hard protective layer, the unevenness is transferred between the protective layer and the soft sound insulating layer. Since it is easy to be formed, it is considered that multiple images are generated.

多重像の発生は、合わせガラス用中間膜の表面に凹凸を形成しなければ防止できる。しかしながら、凹凸を形成しないと、合わせガラスの製造時に充分に脱気することができず、ガラスと中間膜との間に気泡が発生し、合わせガラスの外観を損ねてしまう。 The generation of multiple images can be prevented unless irregularities are formed on the surface of the interlayer film for laminated glass. However, if the unevenness is not formed, the laminated glass cannot be sufficiently degassed at the time of manufacturing, and bubbles are generated between the glass and the interlayer film, which impairs the appearance of the laminated glass.

本発明は、上記現状に鑑み、2層以上の樹脂層が積層された合わせガラス用中間膜であって、合わせガラスの製造工程において優れた脱気性を有し、かつ、多重像の発生を防止できる合わせガラス用中間膜、及び、該合わせガラス用中間膜を含む合わせガラスを提供することを目的とする。 In view of the above situation, the present invention is an interlayer film for laminated glass in which two or more resin layers are laminated, has excellent degassing properties in the manufacturing process of laminated glass, and prevents the generation of multiple images. It is an object of the present invention to provide a laminated glass interlayer film capable of being formed, and a laminated glass including the laminated glass interlayer film.

本発明は、2層以上の樹脂層が積層された合わせガラス用中間膜であって、少なくとも一方の表面に、多数の凹部と多数の凸部とを有し、前記凹部は、底部が連続した溝形状を有し、隣接する前記凹部が平行して規則的に並列しており、前記多数の凹部と多数の凸部とを有する表面は、JIS B−0601(1994)に準拠して測定される凹部の溝深さ(Rzg)が10〜40μmであり、かつ、前記多数の凹部と多数の凸部とを有する表面を有する樹脂層を、該樹脂層が直接接する樹脂層から剥離した後に、剥離した多数の凹部と多数の凸部とを有する表面を有する樹脂層の前記直接接していた樹脂層側の表面をJIS B 0601(1994)に準拠して測定した十点平均粗さ(Rz)が2.7μm未満である合わせガラス用中間膜である。
なお、本発明において、「少なくとも一方の表面に、多数の凹部と多数の凸部とを有し」とは「少なくとも一方の表面に、多数の凹部と多数の凸部とが形成されている」ことをも意味し、「凹部は、底部が連続した溝形状を有し、隣接する前記凹部が平行して規則的に並列しており」とは「凹部は、底部が連続した溝形状を有し、隣接する前記凹部が平行して規則的に形成されている」ことをも意味する。
以下に本発明を詳述する。
The present invention is an interlayer film for laminated glass in which two or more resin layers are laminated, and has a large number of concave portions and a large number of convex portions on at least one surface of the concave portions having a continuous bottom. A surface having a groove shape, the adjacent recesses are parallel and regularly arranged in parallel, and the surface having a large number of concave portions and a large number of convex portions is measured in accordance with JIS B-0601 (1994). After the resin layer having a groove depth (Rzg) of 10 to 40 μm and having a surface having a large number of concave portions and a large number of convex portions is peeled from the resin layer in which the resin layer is in direct contact, the resin layer is peeled off. Ten-point average roughness (Rz) measured in accordance with JIS B 0601 (1994) on the surface of the resin layer having a surface having a large number of peeled concave portions and a large number of convex portions on the resin layer side that was in direct contact with the resin layer. Is an interlayer film for laminated glass having a size of less than 2.7 μm.
In the present invention, "having a large number of concave portions and a large number of convex portions on at least one surface" means "a large number of concave portions and a large number of convex portions are formed on at least one surface". It also means that "the recess has a groove shape with a continuous bottom, and the adjacent recesses are parallel and regularly parallel" means that "the recess has a groove shape with a continuous bottom." However, it also means that the adjacent recesses are regularly formed in parallel. "
The present invention will be described in detail below.

本発明者らは、鋭意検討の結果、合わせガラス用中間膜の表面に形成する凹凸を合わせガラスの製造工程において充分な脱気性を発揮できる程度にする一方、凹凸が形成された表面を有する樹脂層と該樹脂層が直接接する樹脂層との界面に転写される凹凸の粗さを一定以下に抑えることにより、2層以上の樹脂層が積層された合わせガラス用中間膜であっても、合わせガラスの製造時における優れた脱気性と、多重像の発生の防止とを両立できることを見出し、本発明を完成した。 As a result of diligent studies, the present inventors have made the unevenness formed on the surface of the interlayer film for laminated glass to such an extent that sufficient degassing property can be exhibited in the manufacturing process of the laminated glass, while the resin having the surface on which the unevenness is formed. By suppressing the roughness of the unevenness transferred to the interface between the layer and the resin layer in direct contact with the resin layer to a certain level or less, even if it is an interlayer film for laminated glass in which two or more resin layers are laminated, it is laminated. The present invention has been completed by finding that both excellent degassing properties during the production of glass and prevention of the generation of multiple images can be achieved at the same time.

本発明の合わせガラス用中間膜は、少なくとも一方の表面に、多数の凹部と多数の凸部とを有する。これにより、合わせガラスの製造時における脱気性を確保することができる。
上記凹凸は、一方の表面にのみ有してもよいが、著しく脱気性が向上することから、合わせガラス用中間膜の両面に有することが好ましい。
The interlayer film for laminated glass of the present invention has a large number of concave portions and a large number of convex portions on at least one surface. Thereby, the degassing property at the time of manufacturing the laminated glass can be ensured.
The unevenness may be provided only on one surface, but it is preferably provided on both sides of the interlayer film for laminated glass because the degassing property is remarkably improved.

上記凹凸の形状は、少なくとも溝形状を有すればよく、例えば、刻線状、格子状等の、一般的に合わせガラス用中間膜の表面に付与される凹凸の形状を用いることができる。上記凹凸の形状はエンボスロールが転写された形状であってもよい。
また、上記凸部も、図1に示したように頂上部が平面形状であってもよく、図2に示したように平面ではない形状であってもよい。なお、上記凸部の頂上部が平面形状である場合には、該頂上部の平面に更に微細な凹凸が施されていてもよい。
更に、各凹凸の凸部の高さは、同一の高さであってもよいし、異なる高さであってもよく、これらの凸部に対応する凹部の深さも、該凹部の底辺が連続していれば、同一の深さであってもよいし、異なる深さであってもよい。
The shape of the unevenness may be at least a groove shape, and for example, a shape of the unevenness generally given to the surface of the interlayer film for laminated glass, such as a carved line shape or a lattice shape, can be used. The shape of the unevenness may be a shape to which the embossed roll is transferred.
Further, the convex portion may also have a flat top portion as shown in FIG. 1 or a non-planar shape as shown in FIG. When the top of the convex portion has a planar shape, the flat surface of the top may be further provided with fine irregularities.
Further, the heights of the convex portions of each unevenness may be the same height or different heights, and the depths of the concave portions corresponding to these convex portions are also continuous at the bottom of the concave portions. If so, they may have the same depth or different depths.

本発明の合わせガラス用中間膜においては、上記少なくとも一方の表面に有する凹凸の凹部は、底部が連続した溝形状(刻線状)を有し、隣接する前記凹部が平行して規則的に並列している。一般に、2枚のガラス板の間に合わせガラス用中間膜が積層された積層体を圧着するときの空気の抜け易さは、上記凹部の底部の連通性及び平滑性と密接な関係がある。中間膜の少なくとも一方の面の凹凸の形状を刻線状の凹部が平行して規則的に並列する形状とすることにより、上記の底部の連通性はより優れ、著しく脱気性が向上する。
なお、「規則的に並列している」とは、隣接する上記刻線状の凹部が平行して等間隔に並列していてもよく、隣接する上記刻線状の凹部が平行して並列しているが、すべての隣接する上記刻線状の凹部の間隔が等間隔でなくともよいことを意味する。
図1及び図2に、刻線状の凹部が等間隔に平行して並列している合わせガラス用中間膜の一例を表す模式図を示した。
図3に、刻線状の凹部が等間隔ではないが平行して並列している合わせガラス用中間膜の一例を表す模式図を示した。図3において、凹部1と凹部2との間隔Aと、凹部1と凹部3との間隔Bとは異なる。
In the interlayer film for laminated glass of the present invention, the concave-convex recesses on at least one of the surfaces have a groove shape (engraved line shape) with a continuous bottom, and the adjacent recesses are regularly paralleled in parallel. doing. In general, the ease with which air can escape when crimping a laminate in which a laminated glass interlayer film is laminated between two glass plates is closely related to the communication and smoothness of the bottom of the recess. By forming the uneven shape of at least one surface of the interlayer film into a shape in which the engraved concave portions are parallel and regularly arranged, the communication of the bottom portion is more excellent and the degassing property is remarkably improved.
In addition, "regularly parallel" may mean that the adjacent engraved recesses are parallel and parallel at equal intervals, and the adjacent engraved recesses are parallel and parallel. However, it means that the distance between all the adjacent carved linear recesses does not have to be equal.
1 and 2 show a schematic view showing an example of an interlayer film for laminated glass in which engraved linear recesses are arranged in parallel at equal intervals.
FIG. 3 shows a schematic view showing an example of an interlayer film for laminated glass in which engraved linear recesses are arranged in parallel but not at equal intervals. In FIG. 3, the distance A between the recess 1 and the recess 2 and the distance B between the recess 1 and the recess 3 are different.

上記多数の凹部と多数の凸部とを有する表面は、凹部の溝深さ(Rzg)は10〜40μmである。上記溝深さ(Rzg)を10μm以上とすることにより、極めて優れた脱気性を発揮させることができ、40μm以下とすることにより、合わせガラスを製造する際の温度を低くすることができる。上記溝深さ(Rzg)の好ましい下限は15μm、好ましい上限は35μmであり、より好ましい下限は20μm、より好ましい上限は30μmである。
なお、本明細書において凹部の溝深さ(Rzg)とは、JIS B−0601(1994)「表面粗さ−定義及び表示」に規定される、基準長さを2.5mmとし、粗さ曲線の平均線(粗さ曲線までの偏差の2乗和が最小になるように設定した線)を基準とする溝深さを算出し、測定した溝数の溝深さの平均値を意味する。上記溝数は、基準長さを上記凹部の間隔で割った値の小数点以下を切り上げた整数を溝数とする。溝数が5以上である場合には、基準長さに存在する凹部の最も深い順に5箇所の溝深さを算出し、その平均値を基準長さあたりの溝深さとする。溝数が4以下である場合には、基準長さに存在する凹部の最も深い順に、溝数個の溝深さを算出し、その平均値を基準長さあたりの溝深さとする。上記基準長さあたりの溝深さを少なくとも5箇所測定し、その平均値を凹部の溝深さ(Rzg)とする。また、上記溝深さ(Rzg)は、例えば、表面粗さ測定器(小坂研究所社製、SE1700α)等を用いて測定されるデジタル信号をデータ処理することによって容易に得られる。
The surface having a large number of concave portions and a large number of convex portions has a groove depth (Rzg) of the concave portion of 10 to 40 μm. By setting the groove depth (Rzg) to 10 μm or more, extremely excellent degassing property can be exhibited, and by setting it to 40 μm or less, the temperature at the time of manufacturing the laminated glass can be lowered. The preferred lower limit of the groove depth (Rzg) is 15 μm, the preferred upper limit is 35 μm, the more preferred lower limit is 20 μm, and the more preferred upper limit is 30 μm.
In this specification, the groove depth (Rzg) of the recess is defined in JIS B-0601 (1994) "Surface Roughness-Definition and Indication", with a reference length of 2.5 mm and a roughness curve. The groove depth is calculated based on the average line of (the line set so that the sum of squares of the deviations to the roughness curve is minimized), and means the average value of the groove depths of the measured number of grooves. The number of grooves is an integer obtained by dividing the reference length by the distance between the recesses and rounding up to the nearest whole number. When the number of grooves is 5 or more, the groove depths at five locations are calculated in the order of the deepest of the recesses existing in the reference length, and the average value is taken as the groove depth per reference length. When the number of grooves is 4 or less, the depths of several grooves are calculated in the order of the deepest of the recesses existing in the reference length, and the average value is taken as the groove depth per the reference length. The groove depth per the reference length is measured at at least 5 points, and the average value is taken as the groove depth (Rzg) of the recess. Further, the groove depth (Rzg) can be easily obtained by data processing a digital signal measured using, for example, a surface roughness measuring instrument (manufactured by Kosaka Research Institute, SE1700α).

本発明において合わせガラス用中間膜の少なくとも一方の表面に多数の凹部と多数の凸部とを形成する方法としては、例えば、エンボスロール法、カレンダーロール法、異形押出法、メルトフラクチャーを利用した押出リップエンボス法等が挙げられる。なかでも、隣接する該刻線状の凹部が平行して規則的に並列している形状が容易に得られることから、エンボスロール法が好適である。 In the present invention, as a method for forming a large number of concave portions and a large number of convex portions on at least one surface of the interlayer film for laminated glass, for example, an embossing roll method, a calendar roll method, a deformed extrusion method, or extrusion using a melt fracture is used. The lip embossing method and the like can be mentioned. Of these, the embossing roll method is preferable because it is easy to obtain a shape in which the adjacent engraved concave portions are parallel and regularly arranged in parallel.

上記エンボスロール法で用いられるエンボスロールとしては、例えば、金属ロール表面に酸化アルミニウムや酸化珪素等の研削材を用いてブラスト処理を行い、次いで表面の過大ピークを減少させるためにバーチカル研削などを用いてラッピングを行うことにより、ロール表面にエンボス模様(凹凸模様)を有するエンボスロールが挙げられる。他にも、彫刻ミル(マザーミル)を用い、この彫刻ミルのエンボス模様(凹凸模様)を金属ロール表面に転写することにより、ロール表面にエンボス模様(凹凸模様)を有するエンボスロールが挙げられる。更に、エッチング(蝕刻)によりロール表面にエンボス模様(凹凸模様)を有するエンボスロール等が挙げられる。 As the embossing roll used in the above embossing roll method, for example, the surface of the metal roll is blasted with a grinding material such as aluminum oxide or silicon oxide, and then vertical grinding or the like is used to reduce the excessive peak on the surface. An embossed roll having an embossed pattern (unevenness pattern) on the surface of the roll can be mentioned by performing wrapping. Another example is an embossed roll having an embossed pattern (unevenness pattern) on the roll surface by transferring the embossed pattern (unevenness pattern) of the engraving mill to the surface of the metal roll using an engraving mill (mother mill). Further, an embossed roll having an embossed pattern (unevenness pattern) on the roll surface by etching (eching) can be mentioned.

本発明の合わせガラス用中間膜は、上記多数の凹部と多数の凸部とを有する表面を有する樹脂層(以下、「表面凹凸樹脂層」ともいう。)を、該表面凹凸樹脂層が直接接する樹脂層から剥離した後に、剥離した表面凹凸樹脂層の樹脂層と接していた側の表面をJIS B 0601(1994)に準拠して測定した十点平均粗さ(Rz)が2.7μm未満である。
上述のように、多重像の発生等の原因は樹脂層間の界面に転写された凹凸にあるが、樹脂層間の界面の凹凸を直接観察することは極めて困難である。樹脂層間の界面の凹凸を直接観察する代わりに、直接接する樹脂層を剥離し、剥離後の樹脂層の表面の十点平均粗さを測定することで、樹脂層間の界面に転写された凹凸を間接的に評価することができ、この凹凸の粗さを一定未満とすることにより、転写された凹凸に起因する多重像の発生を抑制できる。
図4の合わせガラス用中間膜は、多数の凹部と多数の凸部とを有する表面21を有する樹脂層20と樹脂層10が積層された2層構造の合わせガラス用中間膜である。本発明では、この2層構造の合わせガラス用中間膜の樹脂層10から樹脂層20を剥離した後に、剥離した樹脂層20の樹脂層10と接していた側の表面22の表面の十点平均粗さ(Rz)を測定する。
図5の合わせガラス用中間膜は、多数の凹部と多数の凸部とを有する表面21を有する樹脂層20と樹脂層10と樹脂層30がこの順に積層された3層構造の合わせガラス用中間膜である。本発明では、この3層構造の合わせガラス用中間膜の樹脂層10から樹脂層20を剥離した後に、剥離した樹脂層20の樹脂層10と接していた側の表面22の表面の十点平均粗さ(Rz)を測定する。
In the interlayer film for laminated glass of the present invention, the surface concavo-convex resin layer directly contacts a resin layer having a surface having a large number of concave portions and a large number of convex portions (hereinafter, also referred to as "surface concavo-convex resin layer"). After peeling from the resin layer, the surface on the side of the peeled surface unevenness resin layer that was in contact with the resin layer was measured in accordance with JIS B 0601 (1994) with a ten-point average roughness (Rz) of less than 2.7 μm. is there.
As described above, the cause of the generation of multiple images is the unevenness transferred to the interface between the resin layers, but it is extremely difficult to directly observe the unevenness at the interface between the resin layers. Instead of directly observing the unevenness of the interface between the resin layers, the resin layer in direct contact is peeled off, and the ten-point average roughness of the surface of the resin layer after peeling is measured to obtain the unevenness transferred to the interface between the resin layers. It can be evaluated indirectly, and by setting the roughness of the unevenness to less than a certain level, it is possible to suppress the generation of multiple images due to the transferred unevenness.
The laminated glass interlayer film of FIG. 4 is a laminated glass interlayer film having a two-layer structure in which a resin layer 20 having a surface 21 having a large number of concave portions and a large number of convex portions and a resin layer 10 are laminated. In the present invention, after the resin layer 20 is peeled from the resin layer 10 of the interlayer film for laminated glass having this two-layer structure, the ten-point average of the surface of the surface 22 on the side of the peeled resin layer 20 in contact with the resin layer 10. Roughness (Rz) is measured.
The laminated glass interlayer film of FIG. 5 has a three-layer structure in which a resin layer 20 having a surface 21 having a large number of concave portions and a large number of convex portions, a resin layer 10 and a resin layer 30 are laminated in this order. It is a membrane. In the present invention, after the resin layer 20 is peeled from the resin layer 10 of the interlayer film for laminated glass having this three-layer structure, the ten-point average of the surface of the surface 22 on the side of the peeled resin layer 20 in contact with the resin layer 10. Roughness (Rz) is measured.

上記直接接する樹脂層の剥離は、温度25℃、湿度30%の環境下で速度10〜15cm/sの条件で行う。温度、湿度及び剥離速度を一定とすることにより、測定値のバラツキを抑えることができる。剥離は、この条件を満たす限り機械を用いて行ってもよいし、指を使って手動で行ってもよい。
上記直接接する樹脂層の剥離を行った直後に十点平均粗さを測定すると、測定値にバラツキが発生することがある。従って、十点平均粗さの測定は、温度25℃、湿度30%の環境下に2時間静置した後に行うことが好ましい。
このように一定の条件下で上記表面凹凸樹脂層を剥離し、静置した後に、剥離した表面凹凸樹脂層の樹脂層と接していた側の表面の十点平均粗さを測定する。
なお、本明細書において十点平均粗さとは、JIS B 0601(1994)「表面粗さ−定義及び表示」に規定に準拠して測定されるものである。また、上記十点平均粗さは、例えば、高精度形状測定システム(キーエンス社製「KS−1100」、先端ヘッド型番「LT−9510VM」)等を用いて容易に測定することができる。
The resin layer in direct contact with the resin layer is peeled off under the conditions of a temperature of 25 ° C. and a humidity of 30% at a speed of 10 to 15 cm / s. By keeping the temperature, humidity and peeling speed constant, variations in measured values can be suppressed. The peeling may be performed using a machine as long as this condition is satisfied, or may be performed manually using a finger.
If the ten-point average roughness is measured immediately after the resin layer in direct contact with the resin layer is peeled off, the measured values may vary. Therefore, it is preferable to measure the ten-point average roughness after allowing it to stand for 2 hours in an environment of a temperature of 25 ° C. and a humidity of 30%.
After the surface uneven resin layer is peeled off and allowed to stand under certain conditions in this way, the ten-point average roughness of the surface of the peeled surface uneven resin layer on the side in contact with the resin layer is measured.
In this specification, the ten-point average roughness is measured in accordance with the provisions of JIS B 0601 (1994) "Surface Roughness-Definition and Labeling". Further, the ten-point average roughness can be easily measured by using, for example, a high-precision shape measuring system (“KS-1100” manufactured by KEYENCE CORPORATION, tip head model number “LT-9510VM”) or the like.

上記剥離した表面凹凸樹脂層の樹脂層と接していた側の表面の十点平均粗さは、2.7μm未満である。十点平均粗さを2.7μm未満とすることにより、多重像の発生を抑制することができる。十点平均粗さは、2.3μm以下であることが好ましく、1.9μm以下であることがより好ましく、1.7μm以下であることが更に好ましい。十点平均粗さが上記好ましい上限以下であることにより、多重像の発生をより一層抑制することができる。また、十点平均粗さの下限は特に限定されないが、0.001μm以上であることが好ましい。 The ten-point average roughness of the surface of the peeled surface uneven resin layer on the side in contact with the resin layer is less than 2.7 μm. By setting the ten-point average roughness to less than 2.7 μm, the generation of multiple images can be suppressed. The ten-point average roughness is preferably 2.3 μm or less, more preferably 1.9 μm or less, and further preferably 1.7 μm or less. When the ten-point average roughness is equal to or less than the above-mentioned preferable upper limit, the generation of multiple images can be further suppressed. The lower limit of the ten-point average roughness is not particularly limited, but is preferably 0.001 μm or more.

上記剥離した表面凹凸樹脂層の樹脂層と接していた側の表面の十点平均粗さを2.7μm未満とするには、例えば、(1)表面凹凸樹脂層の厚みを厚くする、(2)表面に有する溝深さ(Rzg)を浅くする、(3)表面に有する隣接する刻線状の凹部の間隔(以下、「凹部の間隔」ともいう。)を狭くすることにより、凹部形成時の圧力を分散する、(4)表面に凹凸を形成する際のプレス圧又はプレス線圧を低くする、等を組み合わせることが挙げられる。 In order to make the ten-point average roughness of the surface of the peeled surface uneven resin layer on the side in contact with the resin layer less than 2.7 μm, for example, (1) increase the thickness of the surface uneven resin layer (2). ) By making the groove depth (Rzg) on the surface shallow, and (3) narrowing the spacing between adjacent engraved recesses on the surface (hereinafter, also referred to as "recess spacing"), when forming the recesses. (4) The press pressure or the press line pressure at the time of forming the unevenness on the surface is lowered, and the like can be combined.

上記表面凹凸樹脂層の厚みを厚くすることにより、エンボスロール等を用いて表面に凹凸を形成する際に、直接接する樹脂層への圧力が軽減し、界面への凹凸の転写を抑制することができる。即ち、上記剥離した表面凹凸樹脂層の樹脂層と接していた側の表面の十点平均粗さを2.7μm未満とするためには、上記表面凹凸樹脂層の厚みも、多層構造とする目的を損ねない範囲で、できる限り厚くすることが好ましい。
上記剥離した表面凹凸樹脂層の樹脂層と接していた側の表面の十点平均粗さを2.7μm未満とするための上記表面凹凸樹脂層の厚みは、上記表面凹凸樹脂層やこれに直接接する樹脂層の材質等によって決まり特に限定されないが、一般的な合わせガラス用中間膜においては100〜500μmが好ましく、300〜500μmがより好ましい。例えば、後述する遮音中間膜において保護層の表面に凹凸を形成する場合においては、該保護層の厚さを100μm以上とすることが好ましい。保護層の厚さを100μm以上とすることにより、界面への凹凸の転写を抑制することができる。上記保護層の厚さは300μm以上であることがより好ましく、400μm以上であることが更に好ましく、450μm以上であることが特に好ましい。上記保護層の厚さの上限については特に限定されないが、充分な遮音性を達成できる程度に遮音層の厚さを確保するためには、実質的には500μmが上限である。
By increasing the thickness of the surface uneven resin layer, when forming irregularities on the surface using an emboss roll or the like, the pressure on the resin layer in direct contact can be reduced and the transfer of the irregularities to the interface can be suppressed. it can. That is, in order to make the ten-point average roughness of the surface of the peeled surface uneven resin layer on the side in contact with the resin layer less than 2.7 μm, the purpose of forming the thickness of the surface uneven resin layer is also a multi-layer structure. It is preferable to make it as thick as possible without damaging it.
The thickness of the surface uneven resin layer for reducing the ten-point average roughness of the surface of the peeled surface uneven resin layer on the side in contact with the resin layer to less than 2.7 μm is the thickness of the surface uneven resin layer or directly to the surface uneven resin layer. It is determined by the material of the resin layer in contact and is not particularly limited, but in a general interlayer film for laminated glass, 100 to 500 μm is preferable, and 300 to 500 μm is more preferable. For example, in the case of forming irregularities on the surface of the protective layer in the sound insulation interlayer film described later, the thickness of the protective layer is preferably 100 μm or more. By setting the thickness of the protective layer to 100 μm or more, it is possible to suppress the transfer of unevenness to the interface. The thickness of the protective layer is more preferably 300 μm or more, further preferably 400 μm or more, and particularly preferably 450 μm or more. The upper limit of the thickness of the protective layer is not particularly limited, but in order to secure the thickness of the sound insulation layer to the extent that sufficient sound insulation can be achieved, the upper limit is substantially 500 μm.

上記剥離した表面凹凸樹脂層の樹脂層と接していた側の表面の十点平均粗さは、溝深さ(Rzg)を浅くすることによっても低減させることができる。上述のように圧着の際に優れた脱気性を発揮するためには、上記溝深さ(Rzg)を10μm以上とする必要があるが、これを満たす範囲においてできる限り上記溝深さを浅くすることにより、樹脂層間の界面への凹凸の転写を抑制できる。 The ten-point average roughness of the surface of the peeled surface uneven resin layer on the side in contact with the resin layer can also be reduced by making the groove depth (Rzg) shallow. As described above, in order to exhibit excellent degassing properties during crimping, the groove depth (Rzg) needs to be 10 μm or more, but the groove depth should be made as shallow as possible within a range satisfying this. This makes it possible to suppress the transfer of unevenness to the interface between the resin layers.

上記剥離した表面凹凸樹脂層の樹脂層と接していた側の表面の十点平均粗さは、刻線状の凹部の間隔を狭くすることによっても低減させることができる。
上記剥離した表面凹凸樹脂層の樹脂層と接していた側の表面の十点平均粗さを2.7μm未満とするための上記刻線状の凹部の間隔は、上記表面凹凸樹脂層やこれに直接接する樹脂層の材質等によって決まり特に限定されないが、一般的な合わせガラス用中間膜においては500μm以下が好ましい。例えば、後述する遮音中間膜において保護層の表面に凹凸を形成する場合において、刻線状の凹部の間隔を500μm以下とすることが好ましい。刻線状の凹部の間隔を500μm以下とすることにより、樹脂層間の界面への凹凸の転写を抑制することができる。上記刻線状の凹部の間隔は、400μm以下であることがより好ましく、300μm以下であることが更に好ましく、250μm以下であることが最も好ましい。上記刻線状の凹部の間隔の下限については特に限定されないが、合わせガラス製造時の作業性の観点から実質的には10μmが下限である。
The ten-point average roughness of the surface of the peeled surface uneven resin layer on the side in contact with the resin layer can also be reduced by narrowing the spacing between the engraved concave portions.
The spacing between the engraved linear recesses so that the average roughness at 10 points on the surface of the peeled surface uneven resin layer on the side in contact with the resin layer is less than 2.7 μm is the same as that of the surface uneven resin layer. It is determined by the material of the resin layer in direct contact and is not particularly limited, but is preferably 500 μm or less in a general interlayer film for laminated glass. For example, in the case of forming irregularities on the surface of the protective layer in the sound insulation interlayer film described later, it is preferable that the distance between the engraved recesses is 500 μm or less. By setting the distance between the engraved recesses to 500 μm or less, it is possible to suppress the transfer of irregularities to the interface between the resin layers. The distance between the engraved recesses is more preferably 400 μm or less, further preferably 300 μm or less, and most preferably 250 μm or less. The lower limit of the interval between the engraved linear recesses is not particularly limited, but from the viewpoint of workability during the production of laminated glass, the lower limit is substantially 10 μm.

なお、本明細書において刻線状の凹部の間隔とは、隣接する刻線状の凹部において該2つの凹部の最底部間の最短距離を意味する。具体的には、上記凹部の間隔は、光学顕微鏡(例えば、SONIC社製、BS−8000III)を用いて、合わせガラス用中間膜の表面(観察範囲20mm×20mm)を観察し、観察された隣接する凹部の最底部間の最短距離をすべて測定する。次いで、測定された最短距離の平均値を算出することにより、凹部の間隔が得られる。また、測定された最短距離の最大値を凹部の間隔としてもよい。凹部の間隔は最短距離の平均値であってもよく、最短距離の最大値であってもよいが、最短距離の平均値であることが好ましい。 In the present specification, the distance between the engraved recesses means the shortest distance between the bottommost portions of the two engraved recesses in the adjacent engraved recesses. Specifically, the spacing between the recesses is determined by observing the surface (observation range 20 mm × 20 mm) of the interlayer film for laminated glass using an optical microscope (for example, BS-8000III manufactured by SONIC) and observing the adjacent portions. Measure all the shortest distances between the bottoms of the recesses. Then, by calculating the average value of the measured shortest distances, the distance between the recesses can be obtained. Further, the maximum value of the measured shortest distance may be used as the distance between the recesses. The distance between the recesses may be the average value of the shortest distances or the maximum value of the shortest distances, but is preferably the average value of the shortest distances.

上記剥離した表面凹凸樹脂層の樹脂層と接していた側の表面の十点平均粗さは、表面に凹凸の形成する際のプレス圧又はプレス線圧を調整することによっても低減させることができる。
例えばエンボスロールを用いて表面に凹凸を形成する場合、転写条件として合わせガラス用中間膜の温度、ロール温度、線速、プレス圧又はプレス線圧を調整する。この際のプレス圧又はプレス線圧等の転写条件を調整することによっても樹脂層間の界面への凹凸の転写を抑制できる。
The ten-point average roughness of the surface of the peeled surface uneven resin layer on the side in contact with the resin layer can also be reduced by adjusting the press pressure or the press linear pressure at the time of forming the irregularities on the surface. ..
For example, when unevenness is formed on the surface by using an embossed roll, the temperature, roll temperature, linear velocity, press pressure or press linear pressure of the laminated glass interlayer film is adjusted as transfer conditions. By adjusting the transfer conditions such as the press pressure or the press linear pressure at this time, the transfer of unevenness to the interface between the resin layers can also be suppressed.

本発明の合わせガラス用中間膜は、2層以上の樹脂層が積層されている。例えば、2層以上の樹脂層として、第1の樹脂層と第2の樹脂層とを有し、かつ、第1の樹脂層と第2の樹脂層とが異なる性質を有することにより、1層だけでは実現が困難であった種々の性能を有する合わせガラス用中間膜を提供することができる。一方、2層以上の樹脂層が積層されている場合、多重像の問題が発生する。 In the interlayer film for laminated glass of the present invention, two or more resin layers are laminated. For example, as two or more resin layers, one layer is provided by having a first resin layer and a second resin layer, and having different properties between the first resin layer and the second resin layer. It is possible to provide an interlayer film for laminated glass having various performances that has been difficult to realize by itself. On the other hand, when two or more resin layers are laminated, the problem of multiple images occurs.

上記樹脂層は熱可塑性樹脂を含むことが好ましい。
上記熱可塑性樹脂として、例えば、ポリフッ化ビニリデン、ポリテトラフルオロエチレン、フッ化ビニリデン−六フッ化プロピレン共重合体、ポリ三フッ化エチレン、アクリロニトリル−ブタジエン−スチレン共重合体、ポリエステル、ポリエーテル、ポリアミド、ポリカーボネート、ポリアクリレート、ポリメタクリレート、ポリ塩化ビニル、ポリエチレン、ポリプロピレン、ポリスチレン、ポリビニルアセタール、エチレン−酢酸ビニル共重合体等が挙げられる。なかでも、上記樹脂層はポリビニルアセタール、又は、エチレン−酢酸ビニル共重合体を含有することが好ましく、ポリビニルアセタールを含有することがより好ましい。
The resin layer preferably contains a thermoplastic resin.
Examples of the thermoplastic resin include polyvinylidene fluoride, polytetrafluoroethylene, vinylidene fluoride-propylene hexafluoride copolymer, polyethylene trifluoride, acrylonitrile-butadiene-styrene copolymer, polyester, polyether, and polyamide. , Polycarbonate, polyacrylate, polymethacrylate, polyvinyl chloride, polyethylene, polypropylene, polystyrene, polyvinyl acetal, ethylene-vinyl acetate copolymer and the like. Among them, the resin layer preferably contains polyvinyl acetal or an ethylene-vinyl acetate copolymer, and more preferably contains polyvinyl acetal.

上記樹脂層は、ポリビニルアセタールと可塑剤とを含むことが好ましい。
上記可塑剤としては、合わせガラス用中間膜に一般的に用いられる可塑剤であれば特に限定されず、例えば、一塩基性有機酸エステル、多塩基性有機酸エステル等の有機可塑剤や、有機リン酸化合物、有機亜リン酸化合物等のリン酸可塑剤等が挙げられる。
上記有機可塑剤として、例えば、トリエチレングリコール−ジ−2−エチルヘキサノエート、トリエチレングリコール−ジ−2−エチルブチレート、トリエチレングリコール−ジ−n−ヘプタノエート、テトラエチレングリコール−ジ−2−エチルヘキサノエート、テトラエチレングリコール−ジ−2−エチルブチレート、テトラエチレングリコール−ジ−n−ヘプタノエート、ジエチレングリコール−ジ−2−エチルヘキサノエート、ジエチレングリコール−ジ−2−エチルブチレート、ジエチレングリコール−ジ−n−ヘプタノエート等が挙げられる。なかでも、上記樹脂層はトリエチレングリコール−ジ−2−エチルヘキサノエート、トリエチレングリコール−ジ−2−エチルブチレート、又は、トリエチレングリコール−ジ−n−ヘプタノエートを含むことが好ましく、トリエチレングリコール−ジ−2−エチルヘキサノエートを含むことがより好ましい。
The resin layer preferably contains polyvinyl acetal and a plasticizer.
The plasticizer is not particularly limited as long as it is a plasticizer generally used for an interlayer film for laminated glass, and for example, an organic plasticizer such as a monobasic organic acid ester or a polybasic organic acid ester, or an organic plasticizer. Examples thereof include phosphoric acid plasticizers such as phosphoric acid compounds and organic phosphite compounds.
Examples of the organic plasticizer include triethylene glycol-di-2-ethylhexanoate, triethylene glycol-di-2-ethylbutyrate, triethylene glycol-di-n-heptanoate, and tetraethylene glycol-di-2. -Ethylene hexanoate, tetraethylene glycol-di-2-ethylbutyrate, tetraethylene glycol-di-n-heptanoate, diethylene glycol-di-2-ethylhexanoate, diethylene glycol-di-2-ethylbutyrate, diethylene glycol -Di-n-heptanoate and the like can be mentioned. Among them, the resin layer preferably contains triethylene glycol-di-2-ethylhexanoate, triethylene glycol-di-2-ethylbutyrate, or triethylene glycol-di-n-heptanoate. More preferably, it contains ethylene glycol-di-2-ethylhexanoate.

上記樹脂層は、接着力調整剤を含有することが好ましい。特に、合わせガラスを製造するときに、ガラスと接触する樹脂層は、上記接着力調整剤を含有することが好ましい。
上記接着力調整剤としては、例えば、アルカリ金属塩又はアルカリ土類金属塩が好適に用いられる。上記接着力調整剤として、例えば、カリウム、ナトリウム、マグネシウム等の塩が挙げられる。
上記塩を構成する酸としては、例えば、オクチル酸、ヘキシル酸、2−エチル酪酸、酪酸、酢酸、蟻酸等のカルボン酸の有機酸、又は、塩酸、硝酸等の無機酸が挙げられる。合わせガラスを製造するときに、ガラスと樹脂層との接着力を容易に調製できることから、ガラスと接触する樹脂層は、接着力調整剤として、マグネシウム塩を含むことが好ましい。
The resin layer preferably contains an adhesive force adjusting agent. In particular, when manufacturing laminated glass, the resin layer that comes into contact with the glass preferably contains the above-mentioned adhesive force adjusting agent.
As the adhesive strength adjusting agent, for example, an alkali metal salt or an alkaline earth metal salt is preferably used. Examples of the adhesive strength adjusting agent include salts of potassium, sodium, magnesium and the like.
Examples of the acid constituting the salt include organic acids of carboxylic acids such as octyl acid, hexic acid, 2-ethylbutyric acid, butyric acid, acetic acid and formic acid, and inorganic acids such as hydrochloric acid and nitric acid. Since the adhesive force between the glass and the resin layer can be easily prepared when the laminated glass is produced, the resin layer in contact with the glass preferably contains a magnesium salt as an adhesive force adjusting agent.

上記樹脂層は、必要に応じて、酸化防止剤、光安定剤、接着力調整剤として変成シリコーンオイル、難燃剤、帯電防止剤、耐湿剤、熱線反射剤、熱線吸収剤等の添加剤を含有してもよい。 The resin layer contains additives such as an antioxidant, a light stabilizer, and a modified silicone oil as an adhesive strength adjusting agent, a flame retardant, an antistatic agent, a moisture resistant agent, a heat ray reflecting agent, and a heat ray absorbing agent, if necessary. You may.

本発明の合わせガラス用中間膜では、2層以上の樹脂層として、少なくとも第1の樹脂層と第2の樹脂層とを有し、上記第1の樹脂層に含まれるポリビニルアセタール(以下、ポリビニルアセタールAという。)の水酸基量が、上記第2の樹脂層に含まれるポリビニルアセタール(以下、ポリビニルアセタールBという。)の水酸基量と異なることが好ましい。
ポリビニルアセタールAとポリビニルアセタールBとの性質が異なるため、1層だけでは実現が困難であった種々の性能を有する合わせガラス用中間膜を提供することができる。例えば、2層の上記第2の樹脂層の間に、上記第1の樹脂層が積層されており、かつ、ポリビニルアセタールAの水酸基量がポリビニルアセタールBの水酸基量より低い場合、上記第1の樹脂層は上記第2の樹脂層と比較してガラス転移温度が低くなる傾向にある。結果として、上記第1の樹脂層が上記第2の樹脂層より軟らかくなり、合わせガラス用中間膜の遮音性が高くなる。また、2層の上記第2の樹脂層の間に、上記第1の樹脂層が積層されており、かつ、ポリビニルアセタールAの水酸基量がポリビニルアセタールBの水酸基量より高い場合、上記第1の樹脂層は上記第2の樹脂層と比較してガラス転移温度が高くなる傾向にある。結果として、上記第1の樹脂層が上記第2の樹脂層より硬くなり、合わせガラス用中間膜の耐貫通性が高くなる。
The interlayer film for laminated glass of the present invention has at least a first resin layer and a second resin layer as two or more resin layers, and a polyvinyl acetal (hereinafter, polyvinyl) contained in the first resin layer. It is preferable that the amount of hydroxyl groups of acetal A) is different from the amount of hydroxyl groups of polyvinyl acetal (hereinafter referred to as polyvinyl acetal B) contained in the second resin layer.
Since the properties of polyvinyl acetal A and polyvinyl acetal B are different, it is possible to provide an interlayer film for laminated glass having various performances that was difficult to realize with only one layer. For example, when the first resin layer is laminated between the two second resin layers and the amount of hydroxyl groups of polyvinyl acetal A is lower than the amount of hydroxyl groups of polyvinyl acetal B, the first The resin layer tends to have a lower glass transition temperature than the second resin layer. As a result, the first resin layer becomes softer than the second resin layer, and the sound insulation of the laminated glass interlayer film becomes high. When the first resin layer is laminated between the two second resin layers and the amount of hydroxyl groups of polyvinyl acetal A is higher than the amount of hydroxyl groups of polyvinyl acetal B, the first The resin layer tends to have a higher glass transition temperature than the second resin layer. As a result, the first resin layer becomes harder than the second resin layer, and the penetration resistance of the laminated glass interlayer film becomes high.

更に、上記第1の樹脂層及び上記第2の樹脂層が可塑剤を含む場合、上記第1の樹脂層におけるポリビニルアセタール100質量部に対する可塑剤の含有量(以下、含有量Aという。)が、上記第2の樹脂層におけるポリビニルアセタール100質量部に対する可塑剤の含有量(以下、含有量Bという。)と異なることが好ましい。例えば、2層の上記第2の樹脂層の間に、上記第1の樹脂層が積層されており、かつ、上記含有量Aが上記含有量Bより多い場合、上記第1の樹脂層は上記第2の樹脂層と比較してガラス転移温度が低くなる傾向にある。結果として、上記第1の樹脂層が上記第2の樹脂層より軟らかくなり、合わせガラス用中間膜の遮音性が高くなる。また、2層の上記第2の樹脂層の間に、上記第1の樹脂層が積層されており、かつ、上記含有量Aが上記含有量Bより少ない場合、上記第1の樹脂層は上記第2の樹脂層と比較してガラス転移温度が高くなる傾向にある。結果として、上記第1の樹脂層が上記第2の樹脂層より硬くなり、合わせガラス用中間膜の耐貫通性が高くなる。 Further, when the first resin layer and the second resin layer contain a plasticizer, the content of the plasticizer in the first resin layer with respect to 100 parts by mass of polyvinyl acetal (hereinafter referred to as content A) is determined. It is preferable that the content of the plasticizer in the second resin layer is different from the content of the plasticizer (hereinafter referred to as the content B) with respect to 100 parts by mass of polyvinyl acetal. For example, when the first resin layer is laminated between the two second resin layers and the content A is larger than the content B, the first resin layer is said. The glass transition temperature tends to be lower than that of the second resin layer. As a result, the first resin layer becomes softer than the second resin layer, and the sound insulation of the laminated glass interlayer film becomes high. Further, when the first resin layer is laminated between the two second resin layers and the content A is smaller than the content B, the first resin layer is described. The glass transition temperature tends to be higher than that of the second resin layer. As a result, the first resin layer becomes harder than the second resin layer, and the penetration resistance of the laminated glass interlayer film becomes high.

本発明の合わせガラス用中間膜を構成する2層以上の樹脂層の組み合わせとしては、例えば、合わせガラスの遮音性を向上させるために、上記第1の樹脂層として遮音層と、上記第2の樹脂層として保護層との組み合わせが挙げられる。合わせガラスの遮音性が向上することから、上記遮音層はポリビニルアセタールXと可塑剤とを含み、上記保護層はポリビニルアセタールYと可塑剤とを含むことが好ましい。更に、2層の上記保護層の間に、上記遮音層が積層されている場合、優れた遮音性を有する合わせガラス用中間膜(以下、遮音中間膜ともいう。)を得ることができる。本願発明では、上記遮音層と上記保護層のように、性質が異なる樹脂層が積層されていても、多重像の発生を防止できる合わせガラス用中間膜を得ることができる。以下、遮音中間膜について、より具体的に説明する。 As a combination of two or more resin layers constituting the interlayer film for laminated glass of the present invention, for example, in order to improve the sound insulation of the laminated glass, the sound insulating layer as the first resin layer and the second resin layer are used. Examples of the resin layer include a combination with a protective layer. Since the sound insulation of the laminated glass is improved, it is preferable that the sound insulation layer contains polyvinyl acetal X and a plasticizer, and the protective layer contains polyvinyl acetal Y and a plasticizer. Further, when the sound insulation layer is laminated between the two protective layers, an interlayer film for laminated glass having excellent sound insulation (hereinafter, also referred to as a sound insulation interlayer film) can be obtained. In the present invention, it is possible to obtain an interlayer film for laminated glass capable of preventing the generation of multiple images even when resin layers having different properties such as the sound insulation layer and the protective layer are laminated. Hereinafter, the sound insulation interlayer film will be described more specifically.

上記遮音中間膜において、上記遮音層は遮音性を付与する役割を有する。
上記遮音層は、ポリビニルアセタールXと可塑剤とを含有することが好ましい。
上記ポリビニルアセタールXは、ポリビニルアルコールをアルデヒドによりアセタール化することにより調製することができる。上記ポリビニルアルコールは、通常、ポリ酢酸ビニルをけん化することにより得られる。
上記ポリビニルアルコールの平均重合度の好ましい下限は200、好ましい上限5000である。上記ポリビニルアルコールの平均重合度を200以上とすることにより、得られる遮音中間膜の耐貫通性を向上させることができ、5000以下とすることにより、遮音層の成形性を確保することができる。上記ポリビニルアルコールの平均重合度のより好ましい下限は500、より好ましい上限は4000である。
なお、上記ポリビニルアルコールの平均重合度は、JIS K6726「ポリビニルアルコール試験方法」に準拠した方法により求められる。
In the sound insulation interlayer film, the sound insulation layer has a role of imparting sound insulation.
The sound insulation layer preferably contains polyvinyl acetal X and a plasticizer.
The polyvinyl acetal X can be prepared by acetalizing polyvinyl alcohol with an aldehyde. The polyvinyl alcohol is usually obtained by saponifying polyvinyl acetate.
The preferable lower limit of the average degree of polymerization of the polyvinyl alcohol is 200, and the preferable upper limit is 5000. By setting the average degree of polymerization of the polyvinyl alcohol to 200 or more, the penetration resistance of the obtained sound insulation interlayer film can be improved, and by setting the average degree of polymerization to 5000 or less, the moldability of the sound insulation layer can be ensured. The more preferable lower limit of the average degree of polymerization of the polyvinyl alcohol is 500, and the more preferable upper limit is 4000.
The average degree of polymerization of the polyvinyl alcohol is determined by a method based on JIS K6726 "polyvinyl alcohol test method".

上記ポリビニルアルコールをアセタール化するためのアルデヒドの炭素数の好ましい下限は4、好ましい上限は6である。アルデヒドの炭素数を4以上とすることにより、充分な量の可塑剤を安定して含有させることができ、優れた遮音性能を発揮することができる。また、可塑剤のブリードアウトを防止することができる。アルデヒドの炭素数を6以下とすることにより、ポリビニルアセタールXの合成を容易にし、生産性を確保できる。
上記炭素数が4〜6のアルデヒドとしては、直鎖状のアルデヒドであってもよいし、分枝状のアルデヒドであってもよく、例えば、n−ブチルアルデヒド、n−バレルアルデヒド等が挙げられる。
The preferable lower limit of the carbon number of the aldehyde for acetalizing the polyvinyl alcohol is 4, and the preferable upper limit is 6. By setting the number of carbon atoms of the aldehyde to 4 or more, a sufficient amount of plasticizer can be stably contained, and excellent sound insulation performance can be exhibited. In addition, bleeding out of the plasticizer can be prevented. By setting the carbon number of the aldehyde to 6 or less, the synthesis of polyvinyl acetal X can be facilitated and the productivity can be ensured.
The aldehyde having 4 to 6 carbon atoms may be a linear aldehyde or a branched aldehyde, and examples thereof include n-butyraldehyde and n-valeraldehyde. ..

上記ポリビニルアセタールXの水酸基量の好ましい上限は30モル%である。上記ポリビニルアセタールXの水酸基量を30モル%以下とすることにより、遮音性を発揮するのに必要な量の可塑剤を含有させることができ、可塑剤のブリードアウトを防止することができる。上記ポリビニルアセタールXの水酸基量のより好ましい上限は28モル%、更に好ましい上限は26モル%、特に好ましい上限は24モル%、好ましい下限は10モル%、より好ましい下限は15モル%、更に好ましい下限は20モル%である。
上記ポリビニルアセタールXの水酸基量は、水酸基が結合しているエチレン基量を、主鎖の全エチレン基量で除算して求めたモル分率を百分率(モル%)で表した値である。上記水酸基が結合しているエチレン基量は、例えば、JIS K6728「ポリビニルブチラール試験方法」に準拠した方法により、上記ポリビニルアセタールXの水酸基が結合しているエチレン基量を測定することにより求めることができる。
The preferable upper limit of the amount of hydroxyl groups of the polyvinyl acetal X is 30 mol%. By setting the amount of hydroxyl groups of the polyvinyl acetal X to 30 mol% or less, an amount of plasticizer necessary for exhibiting sound insulation can be contained, and bleed-out of the plasticizer can be prevented. A more preferable upper limit of the amount of hydroxyl groups of the polyvinyl acetal X is 28 mol%, a further preferable upper limit is 26 mol%, a particularly preferable upper limit is 24 mol%, a preferable lower limit is 10 mol%, a more preferable lower limit is 15 mol%, and a further preferable lower limit. Is 20 mol%.
The amount of hydroxyl groups of the polyvinyl acetal X is a value expressed as a percentage (mol%) of the molar fraction obtained by dividing the amount of ethylene groups to which the hydroxyl groups are bonded by the total amount of ethylene groups in the main chain. The amount of the ethylene group to which the hydroxyl group is bonded can be determined, for example, by measuring the amount of the ethylene group to which the hydroxyl group of the polyvinyl acetal X is bonded by a method based on JIS K6728 “Polyvinyl Butyral Test Method”. it can.

上記ポリビニルアセタールXのアセタール基量の好ましい下限は60モル%、好ましい上限は85モル%である。上記ポリビニルアセタールXのアセタール基量を60モル%以上とすることにより、遮音層の疎水性を高くして、遮音性を発揮するのに必要な量の可塑剤を含有させることができ、可塑剤のブリードアウトや白化を防止することができる。上記ポリビニルアセタールXのアセタール基量を85モル%以下とすることにより、ポリビニルアセタールXの合成を容易にし、生産性を確保することができる。上記ポリビニルアセタールXのアセタール基量の下限は65モル%がより好ましく、68モル%以上が更に好ましい。
上記アセタール基量は、JIS K6728「ポリビニルブチラール試験方法」に準拠した方法により、上記ポリビニルアセタールXのアセタール基が結合しているエチレン基量を測定することにより求めることができる。
The preferable lower limit of the acetal group amount of the polyvinyl acetal X is 60 mol%, and the preferable upper limit is 85 mol%. By setting the acetal group amount of the polyvinyl acetal X to 60 mol% or more, the hydrophobicity of the sound insulation layer can be increased, and an amount of plasticizer necessary for exhibiting sound insulation can be contained, and the plasticizer can be contained. Bleedout and whitening can be prevented. By setting the acetal group amount of the polyvinyl acetal X to 85 mol% or less, the synthesis of the polyvinyl acetal X can be facilitated and the productivity can be ensured. The lower limit of the acetal group amount of the polyvinyl acetal X is more preferably 65 mol%, further preferably 68 mol% or more.
The acetal group amount can be determined by measuring the amount of the ethylene group to which the acetal group of the polyvinyl acetal X is bonded by a method based on JIS K6728 "polyvinyl butyral test method".

上記ポリビニルアセタールXのアセチル基量の好ましい下限は0.1モル%、好ましい上限は30モル%である。上記ポリビニルアセタールXのアセチル基量を0.1モル%以上とすることにより、遮音性を発揮するのに必要な量の可塑剤を含有させることができ、ブリードアウトを防止することができる。また、上記ポリビニルアセタールXのアセチル基量を30モル%以下とすることにより、遮音層の疎水性を高くして、白化を防止することができる。上記アセチル基量のより好ましい下限は1モル%、更に好ましい下限は5モル%、特に好ましい下限は8モル%、より好ましい上限は25モル%、更に好ましい上限は20モル%である。上記アセチル基量は、主鎖の全エチレン基量から、アセタール基が結合しているエチレン基量と、水酸基が結合しているエチレン基量とを差し引いた値を、主鎖の全エチレン基量で除算して求めたモル分率を百分率(モル%)で表した値である。 The preferable lower limit of the acetyl group amount of the polyvinyl acetal X is 0.1 mol%, and the preferable upper limit is 30 mol%. By setting the amount of the acetyl group of the polyvinyl acetal X to 0.1 mol% or more, it is possible to contain an amount of plasticizer necessary for exhibiting sound insulation, and it is possible to prevent bleed-out. Further, by setting the amount of the acetyl group of the polyvinyl acetal X to 30 mol% or less, the hydrophobicity of the sound insulation layer can be increased and whitening can be prevented. The more preferable lower limit of the amount of acetyl groups is 1 mol%, the further preferable lower limit is 5 mol%, the particularly preferable lower limit is 8 mol%, the more preferable upper limit is 25 mol%, and the further preferable upper limit is 20 mol%. The acetyl group amount is the total ethylene group amount of the main chain obtained by subtracting the ethylene group amount to which the acetal group is bonded and the ethylene group amount to which the hydroxyl group is bonded from the total ethylene group amount of the main chain. It is a value expressed as a percentage (mol%) of the molar fraction obtained by dividing by.

特に、上記遮音層に遮音性を発揮するのに必要な量の可塑剤を容易に含有させることができることから、上記ポリビニルアセタールXは、上記アセチル基量が8モル%以上のポリビニルアセタール、又は、上記アセチル基量が8モル%未満、かつ、アセタール基量が65モル%以上のポリビニルアセタールであることが好ましい。また、上記ポリビニルアセタールXは、上記アセチル基量が8モル%以上のポリビニルアセタール、又は、上記アセチル基量が8モル%未満、かつ、アセタール基量が68モル%以上のポリビニルアセタールであることが、より好ましい。 In particular, since the sound insulation layer can easily contain an amount of a plasticizing agent necessary for exhibiting sound insulation, the polyvinyl acetal X is a polyvinyl acetal having an acetyl group content of 8 mol% or more, or It is preferable that the polyvinyl acetal has an acetyl group content of less than 8 mol% and an acetal group content of 65 mol% or more. Further, the polyvinyl acetal X may be a polyvinyl acetal having an acetyl group amount of 8 mol% or more, or a polyvinyl acetal having an acetyl group amount of less than 8 mol% and an acetal group amount of 68 mol% or more. , More preferred.

上記遮音層における可塑剤の含有量は、上記ポリビニルアセタールX100質量部に対する好ましい下限が45質量部、好ましい上限が80質量部である。上記可塑剤の含有量を45質量部以上とすることにより、高い遮音性を発揮することができ、80質量部以下とすることにより、可塑剤のブリードアウトが生じて、合わせガラス用中間膜の透明性や接着性の低下を防止することができる。上記可塑剤の含有量のより好ましい下限は50質量部、更に好ましい下限は55質量部、より好ましい上限は75質量部、更に好ましい上限は70質量部である。 Regarding the content of the plasticizer in the sound insulation layer, the preferable lower limit is 45 parts by mass and the preferable upper limit is 80 parts by mass with respect to 100 parts by mass of the polyvinyl acetal X. When the content of the plasticizer is 45 parts by mass or more, high sound insulation can be exhibited, and when it is 80 parts by mass or less, the plasticizer bleeds out and the interlayer film for laminated glass is formed. It is possible to prevent deterioration of transparency and adhesiveness. The more preferable lower limit of the content of the plasticizer is 50 parts by mass, the more preferable lower limit is 55 parts by mass, the more preferable upper limit is 75 parts by mass, and the further preferable upper limit is 70 parts by mass.

上記遮音層の厚さの好ましい下限は50μmである。上記遮音層の厚さを50μm以上とすることにより、充分な遮音性を発揮することができる。上記遮音層の厚さのより好ましい下限は80μmである。なお、上限は特に限定されないが、合わせガラス用中間膜としての厚さを考慮すると、好ましい上限は300μmである。 The preferable lower limit of the thickness of the sound insulation layer is 50 μm. By setting the thickness of the sound insulation layer to 50 μm or more, sufficient sound insulation can be exhibited. A more preferable lower limit of the thickness of the sound insulation layer is 80 μm. Although the upper limit is not particularly limited, the upper limit is preferably 300 μm in consideration of the thickness of the interlayer film for laminated glass.

上記保護層は、遮音層に含まれる大量の可塑剤がブリードアウトして、合わせガラス用中間膜とガラスとの接着性が低下するのを防止し、また、合わせガラス用中間膜に耐貫通性を付与する役割を有する。
上記保護層は、例えば、ポリビニルアセタールYと可塑剤とを含有することが好ましく、ポリビニルアセタールXより水酸基量が大きいポリビニルアセタールYと可塑剤とを含有することがより好ましい。
The protective layer prevents a large amount of plasticizer contained in the sound insulating layer from bleeding out to reduce the adhesiveness between the laminated glass interlayer film and the glass, and also has penetration resistance to the laminated glass interlayer film. Has the role of granting.
The protective layer preferably contains, for example, polyvinyl acetal Y and a plasticizer, and more preferably contains polyvinyl acetal Y having a larger amount of hydroxyl groups than polyvinyl acetal X and a plasticizer.

上記ポリビニルアセタールYは、ポリビニルアルコールをアルデヒドによりアセタール化することにより調製することができる。
上記ポリビニルアルコールは、通常、ポリ酢酸ビニルをけん化することにより得られる。
また、上記ポリビニルアルコールの平均重合度の好ましい下限は200、好ましい上限は5000である。上記ポリビニルアルコールの平均重合度を200以上とすることにより、合わせガラス用中間膜の耐貫通性を向上させることができ、5000以下とすることにより、保護層の成形性を確保することができる。上記ポリビニルアルコールの平均重合度のより好ましい下限は500、より好ましい上限は4000である。
The polyvinyl acetal Y can be prepared by acetalizing polyvinyl alcohol with an aldehyde.
The polyvinyl alcohol is usually obtained by saponifying polyvinyl acetate.
The preferable lower limit of the average degree of polymerization of the polyvinyl alcohol is 200, and the preferable upper limit is 5000. By setting the average degree of polymerization of the polyvinyl alcohol to 200 or more, the penetration resistance of the interlayer film for laminated glass can be improved, and by setting it to 5000 or less, the moldability of the protective layer can be ensured. The more preferable lower limit of the average degree of polymerization of the polyvinyl alcohol is 500, and the more preferable upper limit is 4000.

上記ポリビニルアルコールをアセタール化するためのアルデヒドの炭素数の好ましい下限は3、好ましい上限は4である。アルデヒドの炭素数を3以上とすることにより、合わせガラス用中間膜の耐貫通性が高くなる。アルデヒドの炭素数を4以下とすることにより、ポリビニルアセタールYの生産性が向上する。
上記炭素数が3〜4のアルデヒドとしては、直鎖状のアルデヒドであってもよいし、分枝状のアルデヒドであってもよく、例えば、n−ブチルアルデヒド等が挙げられる。
The preferable lower limit of the carbon number of the aldehyde for acetalizing the polyvinyl alcohol is 3, and the preferable upper limit is 4. By setting the number of carbon atoms of the aldehyde to 3 or more, the penetration resistance of the interlayer film for laminated glass is increased. By setting the number of carbon atoms of the aldehyde to 4 or less, the productivity of polyvinyl acetal Y is improved.
The aldehyde having 3 to 4 carbon atoms may be a linear aldehyde or a branched aldehyde, and examples thereof include n-butyraldehyde and the like.

上記ポリビニルアセタールYの水酸基量の好ましい上限は33モル%、好ましい下限は28モル%である。上記ポリビニルアセタールYの水酸基量を33モル%以下とすることにより、合わせガラス用中間膜の白化を防止することができる。上記ポリビニルアセタールYの水酸基量を28モル%以上とすることにより、合わせガラス用中間膜の耐貫通性が高くなる。 The preferable upper limit of the amount of hydroxyl groups of the polyvinyl acetal Y is 33 mol%, and the preferable lower limit is 28 mol%. By setting the amount of hydroxyl groups of the polyvinyl acetal Y to 33 mol% or less, whitening of the interlayer film for laminated glass can be prevented. By setting the amount of hydroxyl groups of the polyvinyl acetal Y to 28 mol% or more, the penetration resistance of the interlayer film for laminated glass is increased.

上記ポリビニルアセタールYは、アセタール基量の好ましい下限が60モル%、好ましい上限が80モル%である。上記アセタール基量を60モル%以上とすることにより、充分な耐貫通性を発揮するのに必要な量の可塑剤を含有させることができる。上記アセタール基量を80モル%以下とすることにより、上記保護層とガラスとの接着力を確保することができる。上記アセタール基量のより好ましい下限は65モル%、より好ましい上限は69モル%である。 In the polyvinyl acetal Y, the preferable lower limit of the acetal group amount is 60 mol%, and the preferable upper limit is 80 mol%. By setting the amount of the acetal group to 60 mol% or more, it is possible to contain an amount of plasticizer necessary for exhibiting sufficient penetration resistance. By setting the amount of the acetal group to 80 mol% or less, the adhesive force between the protective layer and the glass can be ensured. The more preferable lower limit of the acetal group amount is 65 mol%, and the more preferable upper limit is 69 mol%.

上記ポリビニルアセタールYのアセチル基量の好ましい上限は7モル%である。上記ポリビニルアセタールYのアセチル基量を7モル%以下とすることにより、保護層の疎水性を高くして、白化を防止することができる。上記アセチル基量のより好ましい上限は2モル%であり、好ましい下限は0.1モル%である。なお、ポリビニルアセタールA、B、及び、Yの水酸基量、アセタール基量、及び、アセチル基量は、ポリビニルアセタールXと同様の方法で測定できる。 The preferable upper limit of the acetyl group amount of the polyvinyl acetal Y is 7 mol%. By setting the amount of the acetyl group of the polyvinyl acetal Y to 7 mol% or less, the hydrophobicity of the protective layer can be increased and whitening can be prevented. The more preferable upper limit of the amount of the acetyl group is 2 mol%, and the preferable lower limit is 0.1 mol%. The amount of hydroxyl groups, the amount of acetal groups, and the amount of acetyl groups of polyvinyl acetals A, B, and Y can be measured by the same method as for polyvinyl acetal X.

上記保護層における可塑剤の含有量は、上記ポリビニルアセタールY100質量部に対する好ましい下限が20質量部、好ましい上限が45質量部である。上記可塑剤の含有量を20質量部以上とすることにより、耐貫通性を確保することができ、45質量部以下とすることにより、可塑剤のブリードアウトを防止して、合わせガラス用中間膜の透明性や接着性の低下を防止することができる。上記可塑剤の含有量のより好ましい下限は30質量部、更に好ましい下限は35質量部、より好ましい上限は43質量部、更に好ましい上限は41質量部である。合わせガラスの遮音性がよりいっそう向上することから、上記保護層における可塑剤の含有量は、上記遮音層における可塑剤の含有量よりも少ないことが好ましい。 Regarding the content of the plasticizer in the protective layer, the preferable lower limit is 20 parts by mass and the preferable upper limit is 45 parts by mass with respect to 100 parts by mass of the polyvinyl acetal Y. By setting the content of the plasticizer to 20 parts by mass or more, penetration resistance can be ensured, and by setting the content to 45 parts by mass or less, bleed-out of the plasticizer is prevented and an interlayer film for laminated glass is prevented. It is possible to prevent deterioration of transparency and adhesiveness of the glass. The more preferable lower limit of the content of the plasticizer is 30 parts by mass, the more preferable lower limit is 35 parts by mass, the more preferable upper limit is 43 parts by mass, and the further preferable upper limit is 41 parts by mass. Since the sound insulation of the laminated glass is further improved, the content of the plasticizer in the protective layer is preferably smaller than the content of the plasticizer in the sound insulation layer.

合わせガラスの遮音性がより一層向上することから、ポリビニルアセタールYの水酸基量はポリビニルアセタールXの水酸基量より大きいことが好ましく、1モル%以上大きいことがより好ましく、5モル%以上大きいことが更に好ましく、8モル%以上大きいことが特に好ましい。ポリビニルアセタールX及びポリビニルアセタールYの水酸基量を調整することにより、上記遮音層及び上記保護層における可塑剤の含有量を制御することができ、上記遮音層のガラス転移温度が低くなる。結果として、合わせガラスの遮音性がより一層向上する。
また、合わせガラスの遮音性がより一層向上することから、上記遮音層におけるポリビニルアセタールX100質量部に対する、可塑剤の含有量(以下、含有量Xともいう。)は、上記保護層におけるポリビニルアセタールY100質量部に対する、可塑剤の含有量(以下、含有量Yともいう。)より多いことが好ましく、5質量部以上多いことがより好ましく、15質量部以上多いことが更に好ましく、20質量部以上多いことが特に好ましい。含有量X及び含有量Yを調整することにより、上記遮音層のガラス転移温度が低くなる。結果として、合わせガラスの遮音性がより一層向上する。
Since the sound insulation of the laminated glass is further improved, the amount of hydroxyl groups of polyvinyl acetal Y is preferably larger than the amount of hydroxyl groups of polyvinyl acetal X, more preferably 1 mol% or more, and further preferably 5 mol% or more. It is preferable, and it is particularly preferable that it is larger than 8 mol%. By adjusting the amounts of hydroxyl groups of polyvinyl acetal X and polyvinyl acetal Y, the content of the plasticizer in the sound insulation layer and the protective layer can be controlled, and the glass transition temperature of the sound insulation layer becomes low. As a result, the sound insulation of the laminated glass is further improved.
Further, since the sound insulation of the laminated glass is further improved, the content of the plasticizer (hereinafter, also referred to as the content X) with respect to 100 parts by mass of the polyvinyl acetal X in the sound insulation layer is the polyvinyl acetal Y100 in the protective layer. It is preferably larger than the content of the plasticizer (hereinafter, also referred to as content Y) with respect to parts by mass, more preferably 5 parts by mass or more, further preferably 15 parts by mass or more, and 20 parts by mass or more. Is particularly preferred. By adjusting the content X and the content Y, the glass transition temperature of the sound insulation layer is lowered. As a result, the sound insulation of the laminated glass is further improved.

上記保護層の厚さは、上記保護層の役割を果たし得る範囲に調整すればよく、特に限定されない。ただし、上記保護層上に凹凸を有する場合には、直接接する上記遮音層との界面への凹凸の転写を抑えられるように、可能な範囲で厚くすることが好ましい。具体的には、上記保護層の厚さの好ましい下限は100μm、より好ましい下限は300μm、更に好ましい下限は400μm、特に好ましい下限は450μmである。上記保護層の厚さの上限については特に限定されないが、充分な遮音性を達成できる程度に遮音層の厚さを確保するためには、実質的には500μm程度が上限である。 The thickness of the protective layer may be adjusted to a range in which it can play the role of the protective layer, and is not particularly limited. However, when the protective layer has irregularities, it is preferable to make the protective layer as thick as possible so that the transfer of the irregularities to the interface with the sound insulation layer in direct contact with the protective layer can be suppressed. Specifically, the preferable lower limit of the thickness of the protective layer is 100 μm, the more preferable lower limit is 300 μm, the further preferable lower limit is 400 μm, and the particularly preferable lower limit is 450 μm. The upper limit of the thickness of the protective layer is not particularly limited, but in order to secure the thickness of the sound insulation layer to the extent that sufficient sound insulation can be achieved, the upper limit is substantially about 500 μm.

上記遮音中間膜を製造する方法としては特に限定されず、例えば、上記遮音層と保護層とを、押し出し法、カレンダー法、プレス法等の通常の製膜法によりシート状に製膜した後、積層する方法等が挙げられる。 The method for producing the sound insulation interlayer film is not particularly limited. For example, the sound insulation layer and the protective layer are formed into a sheet by a usual film forming method such as an extrusion method, a calendar method, or a pressing method. Examples thereof include a method of laminating.

遮音層が2層の保護層の間に積層された合わせガラス用中間膜であって、上記遮音層は、ポリビニルアセタール100質量部に対して可塑剤を45〜80質量部含有し、上記保護層は、ポリビニルアセタール100質量部に対して可塑剤を20〜45質量部含有し、上記保護層の少なくとも一方の表面に、多数の凹部と多数の凸部とを有し、上記凹部は、底部が連続した溝形状を有し、隣接する上記凹部が平行して規則的に並列しており、上記保護層の多数の凹部と多数の凸部とを有する表面は、JIS B−0601(1994)に準拠して測定される凹部の溝深さ(Rzg)が10〜40μmであり、かつ、上記多数の凹部と多数の凸部とを有する表面を有する保護層を遮音層から剥離した後に、剥離した保護層の遮音層側の表面をJIS B 0601(1994)に準拠して測定した十点平均粗さが2.7μm未満である合わせガラス用中間膜もまた、本発明の1つである。
なお、本発明において、「少少なくとも一方の保護層の表面に、多数の凹部と多数の凸部とを有し」とは「少なくとも一方の保護層の表面に、多数の凹部と多数の凸部とが形成されている」ことをも意味し、「凹部は、底部が連続した溝形状を有し、隣接する前記凹部が平行して規則的に並列しており」とは「凹部は、底部が連続した溝形状を有し、隣接する前記凹部が平行して規則的に形成されている」ことをも意味する。
The sound insulating layer is an interlayer film for laminated glass laminated between two protective layers, and the sound insulating layer contains 45 to 80 parts by mass of a plasticizer with respect to 100 parts by mass of polyvinyl acetal, and the protective layer. Contains 20 to 45 parts by mass of a plasticizer with respect to 100 parts by mass of polyvinyl acetal, and has a large number of concave portions and a large number of convex portions on at least one surface of the protective layer. A surface having a continuous groove shape, adjacent recesses parallel to each other and regularly parallel to each other, and having a large number of concave portions and a large number of convex portions of the protective layer is described in JIS B-0601 (1994). The protective layer having a concave groove depth (Rzg) of 10 to 40 μm and having a surface having a large number of concave portions and a large number of convex portions, which is measured in accordance with the above, is peeled off after being peeled from the sound insulation layer. An interlayer film for laminated glass having a ten-point average roughness of less than 2.7 μm measured on the surface of the protective layer on the sound insulation layer side in accordance with JIS B 0601 (1994) is also one of the present inventions.
In the present invention, "having a large number of concave portions and a large number of convex portions on the surface of at least one protective layer" means "having a large number of concave portions and a large number of convex portions on the surface of at least one protective layer". It also means that "and is formed", and "the recess has a groove shape with a continuous bottom, and the adjacent recesses are parallel and regularly parallel" means that "the recess is the bottom. Has a continuous groove shape, and the adjacent recesses are regularly formed in parallel. "

本発明の合わせガラス用中間膜が、一対のガラス板の間に積層されている合わせガラスもまた、本発明の1つである。
上記ガラス板は、一般に使用されている透明板ガラスを使用することができる。例えば、フロート板ガラス、磨き板ガラス、型板ガラス、網入りガラス、線入り板ガラス、着色された板ガラス、熱線吸収ガラス、熱線反射ガラス、グリーンガラス等の無機ガラスが挙げられる。また、ガラスの表面に紫外線遮蔽コート層を有する紫外線遮蔽ガラスも用いることができる。更に、ポリエチレンテレフタレート、ポリカーボネート、ポリアクリレート等の有機プラスチックス板を用いることもできる。
上記ガラス板として、2種類以上のガラス板を用いてもよい。例えば、透明フロート板ガラスと、グリーンガラスのような着色されたガラス板との間に、本発明の合わせガラス用中間膜を積層した合わせガラスが挙げられる。また、上記ガラス板として、2種以上の厚さの異なるガラス板を用いてもよい。
A laminated glass in which the interlayer film for laminated glass of the present invention is laminated between a pair of glass plates is also one of the present inventions.
As the glass plate, a generally used transparent plate glass can be used. For example, inorganic glass such as float plate glass, polished plate glass, template glass, meshed glass, wire-lined plate glass, colored plate glass, heat ray absorbing glass, heat ray reflecting glass, and green glass can be mentioned. Further, an ultraviolet shielding glass having an ultraviolet shielding coating layer on the surface of the glass can also be used. Further, an organic plastic plate such as polyethylene terephthalate, polycarbonate, or polyacrylate can also be used.
Two or more types of glass plates may be used as the glass plate. For example, a laminated glass in which an interlayer film for laminated glass of the present invention is laminated between a transparent float plate glass and a colored glass plate such as green glass can be mentioned. Further, as the glass plate, two or more kinds of glass plates having different thicknesses may be used.

本発明の合わせガラスの製造方法としては特に限定されず、従来公知の製造方法を用いることができる。 The method for producing the laminated glass of the present invention is not particularly limited, and a conventionally known production method can be used.

本発明によれば、2層以上の樹脂層が積層された合わせガラス用中間膜であって、合わせガラスの製造工程において優れた脱気性を有し、かつ、多重像の発生を防止できる合わせガラス用中間膜、及び、該合わせガラス用中間膜を含む合わせガラスを提供することができる。 According to the present invention, it is an interlayer film for laminated glass in which two or more resin layers are laminated, has excellent degassing property in the manufacturing process of laminated glass, and can prevent the generation of multiple images. An interlayer film for use and a laminated glass containing the interlayer film for laminated glass can be provided.

表面に底部が連続した溝形状である凹部が等間隔、かつ、隣接する凹部が平行して並列している合わせガラス用中間膜の一例を表す模式図である。It is a schematic diagram which shows an example of the interlayer film for laminated glass which the recesses having the shape of the groove which the bottom is continuous on the surface are at equal intervals, and the adjacent recesses are parallel and parallel. 表面に底部が連続した溝形状である凹部が等間隔、かつ、隣接する凹部が平行して並列している合わせガラス用中間膜の一例を表す模式図である。It is a schematic diagram which shows an example of the interlayer film for laminated glass which the recesses having the shape of the groove which the bottom is continuous on the surface are at equal intervals, and the adjacent recesses are parallel and parallel. 表面に底部が連続した溝形状である凹部が等間隔ではないが、隣接する凹部が平行して並列している合わせガラス用中間膜の一例を表す模式図である。It is a schematic diagram which shows an example of the interlayer film for laminated glass in which the recesses having a groove shape with a continuous bottom on the surface are not evenly spaced, but adjacent recesses are parallel and parallel. 2層構造の合わせガラス用中間膜において、十点平均粗さ(Rz)を測定する表面を説明する模式図である。It is a schematic diagram explaining the surface for measuring the ten-point average roughness (Rz) in the interlayer film for laminated glass of a two-layer structure. 3層構造の合わせガラス用中間膜において、十点平均粗さ(Rz)を測定する表面を説明する模式図である。It is a schematic diagram explaining the surface for measuring the ten-point average roughness (Rz) in the interlayer film for laminated glass of a three-layer structure.

以下に実施例を挙げて本発明の態様を更に詳しく説明するが、本発明はこれら実施例にのみ限定されない。 Hereinafter, embodiments of the present invention will be described in more detail with reference to examples, but the present invention is not limited to these examples.

(実施例1)
(1)遮音層用樹脂組成物の調製
平均重合度が2400のポリビニルアルコールをn−ブチルアルデヒドでアセタール化することにより得られたポリビニルブチラール(アセチル基量12モル%、ブチラール基量66モル%、水酸基量22モル%)100質量部に対して、可塑剤としてトリエチレングリコール−ジ−2−エチルヘキサノエート(3GO)60質量部を添加し、ミキシングロールで充分に混練し、遮音層用樹脂組成物を得た。
(Example 1)
(1) Preparation of Resin Composition for Sound Insulation Layer Polyvinyl butyral (acetyl group amount 12 mol%, butyral group amount 66 mol%, obtained by acetalizing polyvinyl alcohol having an average degree of polymerization of 2400 with n-butyraldehyde, 60 parts by mass of triethylene glycol-di-2-ethylhexanoate (3GO) was added as a plasticizer to 100 parts by mass of (22 mol% hydroxyl group), and the mixture was sufficiently kneaded with a mixing roll to make a resin for a sound insulation layer. The composition was obtained.

(2)保護層用樹脂組成物の調製
平均重合度が1700のポリビニルアルコールをn−ブチルアルデヒドでアセタール化することにより得られたポリビニルブチラール(アセチル基量1モル%、ブチラール基量69モル%、水酸基量30モル%)100質量部に対して、可塑剤としてトリエチレングリコール−ジ−2−エチルヘキサノエート(3GO)40質量部を添加し、ミキシングロールで充分に混練し、保護層用樹脂組成物を得た。
(2) Preparation of Resin Composition for Protective Layer Polyvinyl butyral (acetyl group amount 1 mol%, butyral group amount 69 mol%, obtained by acetalizing polyvinyl alcohol having an average degree of polymerization of 1700 with n-butyraldehyde, To 100 parts by mass of (30 mol% hydroxyl group), 40 parts by mass of triethylene glycol-di-2-ethylhexanoate (3GO) was added as a plasticizer, and the mixture was sufficiently kneaded with a mixing roll to form a protective layer resin. The composition was obtained.

(3)合わせガラス用中間膜の作製
得られた遮音層用樹脂組成物と保護層用樹脂組成物を、共押出機を用いて共押出することにより、保護層用樹脂組成物からなる厚さ450μmのA層(保護層)、遮音層用樹脂組成物からなる厚さ100μmのB層(遮音層)及び保護層用樹脂組成物からなる厚さ450μmのC層(保護層)がこの順に積層された3層構造の合わせガラス用中間膜(遮音中間膜)を得た。
(3) Preparation of Laminated Glass Intermediate Film The obtained resin composition for sound insulation layer and resin composition for protective layer are coextruded using a coextruder to obtain a thickness of the resin composition for protective layer. A 450 μm A layer (protective layer), a 100 μm thick B layer (sound insulation layer) composed of a sound insulation layer resin composition, and a 450 μm thick C layer (protective layer) composed of a protective layer resin composition are laminated in this order. An interlayer film for laminated glass (sound insulation interlayer film) having a three-layer structure was obtained.

(4)凹凸の付与
第1の工程として、下記の手順により合わせガラス用中間膜の両面にランダムな凹凸形状を転写した。まず、鉄ロール表面に、ブラスト剤を用いてランダムな凹凸を施した後、該鉄ロールをバーチカル研削し、更に、より微細なブラスト剤を用いて研削後の平坦部に微細な凹凸を施すことにより、粗大なメインエンボスと微細なサブエンボスをもつ同形状の1対のロールを得た。該1対のロールを凹凸形状転写装置として用い、得られた合わせガラス用中間膜の両面にランダムな凹凸形状を転写した。この時の転写条件として、合わせガラス用中間膜の温度を80℃、上記ロールの温度を145℃、線速を10m/min、プレス線圧を10〜200kN/mとした。賦型後の合わせガラス用中間膜の表面粗さはJIS B 0601(1994)の十点平均粗さRzで測定した結果、16μmであった。測定は表面粗さ測定器(小坂研究所社製、SE1700α)を用いて測定されるデジタル信号をデータ処理することによって得た。測定方向は刻線に対して垂直方向とし、カットオフ値=2.5mm、基準長さ=2.5mm、評価長さ=12.5mm、触針の先端半径=2μm、先端角度=60°、測定速度=0.5mm/sの条件で測定を行った。
(4) Addition of Concavo-convexness As the first step, a random concavo-convex shape was transferred to both sides of the interlayer film for laminated glass by the following procedure. First, the surface of the iron roll is subjected to random irregularities using a blasting agent, then the iron roll is vertically ground, and further, fine irregularities are applied to the flat portion after grinding using a finer blasting agent. Obtained a pair of rolls of the same shape with coarse main embossing and fine sub-embossing. Using the pair of rolls as a concave-convex shape transfer device, a random uneven shape was transferred to both sides of the obtained interlayer film for laminated glass. As the transfer conditions at this time, the temperature of the interlayer film for laminated glass was 80 ° C., the temperature of the roll was 145 ° C., the linear velocity was 10 m / min, and the press linear pressure was 10 to 200 kN / m. The surface roughness of the interlayer film for laminated glass after molding was 16 μm as a result of measurement with a ten-point average roughness Rz of JIS B 0601 (1994). The measurement was obtained by processing the digital signal measured using a surface roughness measuring instrument (manufactured by Kosaka Laboratory Co., Ltd., SE1700α). The measurement direction is perpendicular to the engraved line, cutoff value = 2.5 mm, reference length = 2.5 mm, evaluation length = 12.5 mm, stylus tip radius = 2 μm, tip angle = 60 °, The measurement was performed under the condition of measurement speed = 0.5 mm / s.

第2の工程として、下記の手順により合わせガラス用中間膜の表面に底部が連続した溝形状(刻線状)の凹凸を付与した。三角形斜線型ミルを用いて表面にミル加工を施した金属ロールと45〜75のJIS硬度を有するゴムロールとからなる一対のロールを凹凸形状転写装置として用い、第1の工程でランダムな凹凸形状を転写した合わせガラス用中間膜をこの凹凸形状転写装置に通し、合わせガラス用中間膜のA層の表面に底部が連続した溝形状(刻線状)である凹部が平行して等間隔に並列した凹凸を付与した。このときの転写条件として、合わせガラス用中間膜の温度を常温、ロール温度を130℃、線速を10m/min、膜幅を1.5m、プレス圧を500kPaとした。
次いで、合わせガラス用中間膜のC層の表面に、凹凸形状の異なる金属ロールを用いた以外は上記と同様の操作を施し、底部が連続した溝形状(刻線状)の凹部を付与した。その際、A層の表面に付与した底部が連続した溝形状(刻線状)の凹部と、C層の表面に付与した底部が連続した溝形状(刻線状)の凹部との交差角度が10°となるようにした。
As a second step, the surface of the interlayer film for laminated glass was provided with groove-shaped (engraved line-shaped) irregularities having a continuous bottom portion by the following procedure. A pair of rolls consisting of a metal roll whose surface has been milled using a triangular diagonal line type mill and a rubber roll having a JIS hardness of 45 to 75 is used as a concave-convex shape transfer device, and a random uneven shape is formed in the first step. The transferred interlayer film for laminated glass was passed through this concave-convex shape transfer device, and recesses having a continuous groove shape (engraved line shape) at the bottom were arranged in parallel at equal intervals on the surface of the A layer of the interlayer film for laminated glass. Unevenness was added. As the transfer conditions at this time, the temperature of the interlayer film for laminated glass was room temperature, the roll temperature was 130 ° C., the linear velocity was 10 m / min, the film width was 1.5 m, and the press pressure was 500 kPa.
Next, the same operation as described above was performed on the surface of the C layer of the interlayer film for laminated glass except that metal rolls having different uneven shapes were used to provide recesses having a continuous groove shape (engraved line shape) at the bottom. At that time, the angle of intersection between the groove-shaped (engraved) recess with a continuous bottom provided on the surface of the A layer and the groove-shaped (engraved) recess with a continuous bottom provided on the surface of the C layer It was set to 10 °.

(5)A層及びC層表面の凹凸の測定
光学顕微鏡(SONIC社製、BS−8000III)を用いて、得られた合わせガラス用中間膜のA層及びC層の表面(観察範囲20mm×20mm)を観察し、隣接する凹部の間隔を測定したうえで、隣接する凹部の最底部間の最短距離の平均値を算出することにより、凹部の間隔を得た。A層の表面の凹部の間隔は500μm、C層の表面の凹部の間隔は750μmであった。なお、上記最短距離の平均値及び最大値はいずれも同一であった。
また、得られた合わせガラス用中間膜のA層及びC層の表面の凹部の溝深さ(Rzg)は、JIS B−0601(1994)「表面粗さ−定義及び表示」に規定される、基準長さを2.5mmとし、粗さ曲線の平均線(粗さ曲線までの偏差の2乗和が最小になるように設定した線)を基準とする溝深さを算出し、測定した溝数の溝深さの平均値を基準長さあたりの溝深さとし、基準長さあたりの溝深さの5箇所の平均値とした。上記A層の溝数は5、上記C層の溝数は4であった。また、A層及びC層の表面の上記凹部の溝深さ(Rzg)は、表面粗さ測定器(小坂研究所社製、SE1700α)を用いて測定されるデジタル信号をデータ処理することによって得た。測定方向は刻線に対して垂直方向とし、触針の先端半径=2μm、先端角度=60°、測定速度=0.5mm/sの条件で測定を行った。
A層の表面の凹部の溝深さ(Rzg)は21μm、C層の表面の凹部の溝深さ(Rzg)は19μmであった。
更に、得られた合わせガラス用中間膜のA層及びC層の表面を、表面粗さ測定器(小坂研究所社製、SE1700α)を用いて測定し、十点平均粗さ(Rz)を得た。A層の表面の十点平均粗さ(Rz)は51μm、C層の表面の十点平均粗さ(Rz)は50μmであった。
(5) Measurement of unevenness on the surfaces of layers A and C Using an optical microscope (manufactured by SONIC, BS-8000III), the surfaces of layers A and C (observation range 20 mm × 20 mm) of the obtained interlayer film for laminated glass. ) Was observed, the distance between the adjacent recesses was measured, and then the average value of the shortest distances between the bottoms of the adjacent recesses was calculated to obtain the distance between the recesses. The distance between the recesses on the surface of the A layer was 500 μm, and the distance between the recesses on the surface of the C layer was 750 μm. The average value and the maximum value of the shortest distance were the same.
Further, the groove depth (Rzg) of the recesses on the surfaces of the A layer and the C layer of the obtained interlayer film for laminated glass is defined in JIS B-0601 (1994) "Surface Roughness-Definition and Indication". The groove depth is calculated and measured with the reference length set to 2.5 mm and the groove depth is calculated based on the average line of the roughness curve (the line set so that the sum of squares of the deviations to the roughness curve is minimized). The average value of the groove depths of the numbers was defined as the groove depth per reference length, and the average value of the groove depths per reference length at five locations was used. The number of grooves in the A layer was 5, and the number of grooves in the C layer was 4. Further, the groove depth (Rzg) of the recesses on the surfaces of the A layer and the C layer can be obtained by data processing a digital signal measured using a surface roughness measuring instrument (manufactured by Kosaka Research Institute, SE1700α). It was. The measurement direction was perpendicular to the engraved line, and the measurement was performed under the conditions of the tip radius of the stylus = 2 μm, the tip angle = 60 °, and the measurement speed = 0.5 mm / s.
The groove depth (Rzg) of the concave portion on the surface of the A layer was 21 μm, and the groove depth (Rzg) of the concave portion on the surface of the C layer was 19 μm.
Further, the surfaces of the A layer and the C layer of the obtained laminated glass interlayer film were measured using a surface roughness measuring instrument (SE1700α manufactured by Kosaka Research Institute) to obtain a ten-point average roughness (Rz). It was. The ten-point average roughness (Rz) of the surface of the A layer was 51 μm, and the ten-point average roughness (Rz) of the surface of the C layer was 50 μm.

(6)界面の凹凸の測定
得られた合わせガラス用中間膜を、縦5cm×横5cmに切り出し、温度25℃、湿度30%の環境下に2時間静置した。
A層とB層との間に指を入れ、10〜15cm/sの速度で剥離した。剥離後、更に温度25℃、湿度30%の環境下に2時間静置した。その後、剥離したA層のB層側の表面を、JIS B 0601(1994)に準拠し、高精度形状測定システム(キーエンス社製、「KS−1100」先端ヘッド型番「LT−9510VM」)を用いて測定し、十点平均粗さ(Rz)を得た。剥離したA層のB層側の表面の十点平均粗さ(Rz)は1.7μmであった。測定条件は、ステージ移動速度は100.0μm/s、X軸の測定ピッチを2.0μm、Y軸の測定ピッチを2.0μmに設定する。
B層とC層の間についても同様の方法により剥離し、剥離したC層のB層側の表面の十点平均粗さ(Rz)を得た。剥離したC層のB層側の表面の十点平均粗さ(Rz)は1.9μmであった。
(6) Measurement of Interface Concavities and Conditions The obtained interlayer film for laminated glass was cut out into a length of 5 cm and a width of 5 cm, and allowed to stand in an environment of a temperature of 25 ° C. and a humidity of 30% for 2 hours.
A finger was placed between the A layer and the B layer, and the mixture was peeled off at a speed of 10 to 15 cm / s. After peeling, the mixture was allowed to stand for 2 hours in an environment with a temperature of 25 ° C. and a humidity of 30%. After that, the surface of the peeled A layer on the B layer side was subjected to a high-precision shape measurement system (manufactured by KEYENCE, "KS-1100", tip head model number "LT-9510VM") in accordance with JIS B 0601 (1994). The average roughness (Rz) at 10 points was obtained. The ten-point average roughness (Rz) of the surface of the peeled A layer on the B layer side was 1.7 μm. The measurement conditions are such that the stage moving speed is set to 100.0 μm / s, the X-axis measurement pitch is set to 2.0 μm, and the Y-axis measurement pitch is set to 2.0 μm.
The area between the B layer and the C layer was also peeled by the same method, and the ten-point average roughness (Rz) of the surface of the peeled C layer on the B layer side was obtained. The ten-point average roughness (Rz) of the surface of the peeled C layer on the B layer side was 1.9 μm.

(実施例2〜5、比較例1)
各層の厚さと、A層及びC層表面の凹部の間隔、凹部の溝深さ(Rzg)、十点平均粗さ(Rz)と、剥離したA層のB層側の表面及び剥離したC層のB層側の表面の十点平均粗さ(Rz)とを表1に示したようにした以外は、実施例1と同様の方法により合わせガラス用中間膜を作製した。
実施例2においては、凹凸の付与時の転写条件を、合わせガラス用中間膜の温度を常温、ロール温度を130℃、線速を10m/分、膜幅を1.5m、プレス圧を200kPaとした。
実施例3においては、凹凸の付与時の転写条件を、合わせガラス用中間膜の温度を常温、ロール温度を130℃、線速を10m/分、膜幅を1.5m、プレス圧を400kPaとした。
実施例4においては、凹凸の付与時の転写条件を、合わせガラス用中間膜の温度を常温、ロール温度を130℃、線速を10m/分、膜幅を1.5m、プレス圧を500kPaとした。
実施例5においては、凹凸の付与時の転写条件を、合わせガラス用中間膜の温度を常温、ロール温度を130℃、線速を10m/分、膜幅を1.5m、プレス圧を500kPaとした。
比較例1においては、凹凸の付与時の転写条件を、合わせガラス用中間膜の温度を常温、ロール温度を130℃、線速を10m/分、膜幅を1.5m、プレス圧を200kPaとした。
なお、実施例2〜5及び比較例1の凹部の間隔の測定において、上記凹部の最短距離の平均値及び最大値はいずれも同一であった。
(Examples 2 to 5, Comparative Example 1)
The thickness of each layer, the distance between the recesses on the surfaces of the A and C layers, the groove depth (Rzg) of the recesses, the ten-point average roughness (Rz), the surface of the peeled A layer on the B layer side, and the peeled C layer. An interlayer film for laminated glass was prepared by the same method as in Example 1 except that the ten-point average roughness (Rz) of the surface on the B layer side was as shown in Table 1.
In Example 2, the transfer conditions at the time of imparting unevenness were as follows: the temperature of the interlayer film for laminated glass was room temperature, the roll temperature was 130 ° C., the linear velocity was 10 m / min, the film width was 1.5 m, and the press pressure was 200 kPa. did.
In Example 3, the transfer conditions at the time of imparting unevenness were as follows: the temperature of the interlayer film for laminated glass was room temperature, the roll temperature was 130 ° C., the linear velocity was 10 m / min, the film width was 1.5 m, and the press pressure was 400 kPa. did.
In Example 4, the transfer conditions at the time of imparting unevenness were as follows: the temperature of the interlayer film for laminated glass was room temperature, the roll temperature was 130 ° C., the linear velocity was 10 m / min, the film width was 1.5 m, and the press pressure was 500 kPa. did.
In Example 5, the transfer conditions at the time of imparting unevenness were as follows: the temperature of the interlayer film for laminated glass was room temperature, the roll temperature was 130 ° C., the linear velocity was 10 m / min, the film width was 1.5 m, and the press pressure was 500 kPa. did.
In Comparative Example 1, the transfer conditions at the time of imparting unevenness were as follows: the temperature of the interlayer film for laminated glass was room temperature, the roll temperature was 130 ° C., the linear velocity was 10 m / min, the film width was 1.5 m, and the press pressure was 200 kPa. did.
In the measurement of the distance between the recesses of Examples 2 to 5 and Comparative Example 1, the average value and the maximum value of the shortest distances of the recesses were the same.

(実施例6、7、比較例2)
各層の厚さと、A層及びC層表面の凹部の間隔、凹部の溝深さ(Rzg)、十点平均粗さ(Rz)と、剥離したA層のB層側の表面及び剥離したC層のB層側の表面の十点平均粗さ(Rz)とを表1に示したようにし、凹凸の付与時の転写条件を変更したこと以外は、実施例1と同様の方法により合わせガラス用中間膜を作製した。
実施例6においては、凹凸の付与時の転写条件を、合わせガラス用中間膜の温度を常温、ロール温度を130℃、線速を10m/分、膜幅を1.5m、プレス圧を700kPaとした。
実施例7においては、凹凸の付与時の転写条件を、合わせガラス用中間膜の温度を常温、ロール温度を130℃、線速を10m/分、膜幅を1.5m、プレス圧を200kPaとした。
比較例2においては、凹凸の付与時の転写条件を、合わせガラス用中間膜の温度を常温、ロール温度を130℃、線速を10m/分、膜幅を1.5m、プレス圧を100kPaとした。
なお、実施例6、7及び比較例2の凹部の間隔の測定において、上記凹部の最短距離の平均値及び最大値はいずれも同一であった。
(Examples 6 and 7, Comparative Example 2)
The thickness of each layer, the distance between the recesses on the surfaces of the A and C layers, the groove depth (Rzg) of the recesses, the ten-point average roughness (Rz), the surface of the peeled A layer on the B layer side, and the peeled C layer. The ten-point average roughness (Rz) of the surface on the B layer side of No. 1 is as shown in Table 1, and for laminated glass by the same method as in Example 1 except that the transfer conditions at the time of imparting unevenness are changed. An interlayer film was prepared.
In Example 6, the transfer conditions at the time of imparting unevenness were as follows: the temperature of the interlayer film for laminated glass was room temperature, the roll temperature was 130 ° C., the linear velocity was 10 m / min, the film width was 1.5 m, and the press pressure was 700 kPa. did.
In Example 7, the transfer conditions at the time of imparting unevenness were as follows: the temperature of the interlayer film for laminated glass was room temperature, the roll temperature was 130 ° C., the linear velocity was 10 m / min, the film width was 1.5 m, and the press pressure was 200 kPa. did.
In Comparative Example 2, the transfer conditions at the time of imparting unevenness were as follows: the temperature of the interlayer film for laminated glass was room temperature, the roll temperature was 130 ° C., the linear velocity was 10 m / min, the film width was 1.5 m, and the press pressure was 100 kPa. did.
In the measurement of the distance between the recesses of Examples 6 and 7 and Comparative Example 2, the average value and the maximum value of the shortest distances of the recesses were the same.

(比較例3、4)
酸化アルミニウム(#36:飽和条件で65μm粗さとなる条件)からなるブラスト材を吐出圧力50×10Paで吐出してブラスト処理を行った2本一対のロールを、ゆず肌状(オレンジピール状)のエンボス転写装置として用いた。実施例1で得られた合わせガラス用中間膜をこのゆず肌状(オレンジピール状)のエンボス転写装置に通し、合わせガラス用中間膜のA層及びC層の表面にゆず肌状(オレンジピール状)のエンボスを形成した。
このときの転写条件として、合わせガラス用中間膜の温度を常温、ロール温度を130℃、線速を10m/分、膜幅を1.5m、プレス圧を500kPaとした。
なお、比較例3及び4で得られた合わせガラス用中間膜については、溝深さ(Rzg)を測定することができなかった。
(Comparative Examples 3 and 4)
A pair of rolls that have been blasted by ejecting a blast material made of aluminum oxide (# 36: a condition that gives a roughness of 65 μm under saturation conditions) at a discharge pressure of 50 × 10 4 Pa are formed into a yuzu skin shape (orange peel shape). ) Was used as an embossed transfer device. The interlayer film for laminated glass obtained in Example 1 is passed through this embossed transfer device having a yuzu-skin shape (orange peel shape), and the surface of the layers A and C of the interlayer film for laminated glass has a yuzu-skin shape (orange peel shape). ) Was formed.
As the transfer conditions at this time, the temperature of the interlayer film for laminated glass was room temperature, the roll temperature was 130 ° C., the linear velocity was 10 m / min, the film width was 1.5 m, and the press pressure was 500 kPa.
The groove depth (Rzg) could not be measured for the laminated glass interlayer films obtained in Comparative Examples 3 and 4.

(実施例8〜10)
各層の厚さと、A層及びC層表面の凹部の間隔、凹部の溝深さ(Rzg)、十点平均粗さ(Rz)と、剥離したA層のB層側の表面及び剥離したC層のB層側の表面の十点平均粗さ(Rz)とを表1に示したようにした以外は、実施例1と同様の方法により合わせガラス用中間膜を作製した。
実施例8においては、凹凸の付与時の転写条件を、合わせガラス用中間膜の温度を常温、ロール温度を130℃、線速を10m/分、膜幅を1.5m、プレス圧を200kPaとした。
実施例9においては、凹凸の付与時の転写条件を、合わせガラス用中間膜の温度を常温、ロール温度を130℃、線速を10m/分、膜幅を1.5m、プレス圧を500kPaとした。
実施例10においては、凹凸の付与時の転写条件を、合わせガラス用中間膜の温度を常温、ロール温度を130℃、線速を10m/分、膜幅を1.5m、プレス圧を500kPaとした。
なお、実施例8〜10の凹部の間隔の測定において、上記凹部の最短距離の平均値及び最大値はいずれも同一であった。
(Examples 8 to 10)
The thickness of each layer, the distance between the recesses on the surfaces of the A and C layers, the groove depth (Rzg) of the recesses, the ten-point average roughness (Rz), the surface of the peeled A layer on the B layer side, and the peeled C layer. An interlayer film for laminated glass was prepared by the same method as in Example 1 except that the ten-point average roughness (Rz) of the surface on the B layer side was as shown in Table 1.
In Example 8, the transfer conditions at the time of imparting unevenness were as follows: the temperature of the interlayer film for laminated glass was room temperature, the roll temperature was 130 ° C., the linear velocity was 10 m / min, the film width was 1.5 m, and the press pressure was 200 kPa. did.
In Example 9, the transfer conditions at the time of imparting unevenness were as follows: the temperature of the interlayer film for laminated glass was room temperature, the roll temperature was 130 ° C., the linear velocity was 10 m / min, the film width was 1.5 m, and the press pressure was 500 kPa. did.
In Example 10, the transfer conditions at the time of imparting unevenness were as follows: the temperature of the interlayer film for laminated glass was room temperature, the roll temperature was 130 ° C., the linear velocity was 10 m / min, the film width was 1.5 m, and the press pressure was 500 kPa. did.
In the measurement of the distance between the recesses of Examples 8 to 10, the average value and the maximum value of the shortest distances of the recesses were the same.

(実施例11〜14)
保護層及び遮音層に用いられるポリビニルブチラールのアセチル基量、ブチラール基量及び水酸基量と、可塑剤の含有量とを表1に示すように変更し、各層の厚さと、A層及びC層表面の凹部の間隔、凹部の溝深さ(Rzg)、十点平均粗さ(Rz)と、剥離したA層のB層側の表面及び剥離したC層のB層側の表面の十点平均粗さ(Rz)とを表1に示したようにし、凹凸の付与時の転写条件を変更したこと以外は、実施例1と同様の方法により合わせガラス用中間膜を作製した。なお、保護層及び遮音層に用いられるポリビニルブチラールは、平均重合度が1700のポリビニルアルコールをn−ブチルアルデヒドでアセタール化することにより得た。
実施例11においては、凹凸の付与時の転写条件を、合わせガラス用中間膜の温度を常温、ロール温度を130℃、線速を10m/分、膜幅を1.5m、プレス線圧を200kPaとした。
実施例12においては、凹凸の付与時の転写条件を、合わせガラス用中間膜の温度を常温、ロール温度を130℃、線速を10m/分、膜幅を1.5m、プレス線圧を500kPaとした。
実施例13においては、凹凸の付与時の転写条件を、合わせガラス用中間膜の温度を常温、ロール温度を130℃、線速を10m/分、膜幅を1.5m、プレス線圧を500kPaとした。
実施例14においては、凹凸の付与時の転写条件を、合わせガラス用中間膜の温度を常温、ロール温度を130℃、線速を10m/分、膜幅を1.5m、プレス線圧を550kPaとした。
なお、実施例11〜14の凹部の間隔の測定において、上記凹部の最短距離の平均値及び最大値はいずれも同一であった。
(Examples 11 to 14)
The acetyl group amount, butyral group amount and hydroxyl group amount of polyvinyl butyral used for the protective layer and the sound insulation layer and the content of the plasticizer were changed as shown in Table 1, and the thickness of each layer and the surfaces of the A layer and the C layer were changed. The spacing between the recesses, the groove depth (Rzg) of the recesses, the ten-point average roughness (Rz), and the ten-point average roughness of the peeled A layer on the B layer side and the peeled C layer on the B layer side. (Rz) was as shown in Table 1, and an interlayer film for laminated glass was prepared by the same method as in Example 1 except that the transfer conditions at the time of imparting unevenness were changed. The polyvinyl butyral used for the protective layer and the sound insulating layer was obtained by acetalizing polyvinyl alcohol having an average degree of polymerization of 1700 with n-butyraldehyde.
In Example 11, the transfer conditions at the time of imparting unevenness were as follows: the temperature of the interlayer film for laminated glass was room temperature, the roll temperature was 130 ° C., the linear velocity was 10 m / min, the film width was 1.5 m, and the press linear pressure was 200 kPa. And said.
In Example 12, the transfer conditions at the time of imparting unevenness were as follows: the temperature of the interlayer film for laminated glass was room temperature, the roll temperature was 130 ° C., the linear velocity was 10 m / min, the film width was 1.5 m, and the press linear pressure was 500 kPa. And said.
In Example 13, the transfer conditions at the time of imparting unevenness were as follows: the temperature of the interlayer film for laminated glass was room temperature, the roll temperature was 130 ° C., the linear velocity was 10 m / min, the film width was 1.5 m, and the press linear pressure was 500 kPa. And said.
In Example 14, the transfer conditions at the time of imparting unevenness were as follows: the temperature of the interlayer film for laminated glass was room temperature, the roll temperature was 130 ° C., the linear velocity was 10 m / min, the film width was 1.5 m, and the press linear pressure was 550 kPa. And said.
In the measurement of the distance between the recesses of Examples 11 to 14, the average value and the maximum value of the shortest distances of the recesses were the same.

(評価)
実施例及び比較例で得られた合わせガラス用中間膜について、以下の方法により評価を行った。
結果を表1に示した。なお、表中のBu化度はブチラール基量を、OH化度は水酸基量を、Ac化度はアセチル基量を、可塑剤部数はポリビニルブチラール100質量部に対する可塑剤の含有量を、それぞれ示す。
(Evaluation)
The interlayer films for laminated glass obtained in Examples and Comparative Examples were evaluated by the following methods.
The results are shown in Table 1. In the table, the degree of Bu conversion indicates the amount of butyral group, the degree of OH conversion indicates the amount of hydroxyl group, the degree of Ac conversion indicates the amount of acetyl group, and the number of plasticizer parts indicates the content of the plasticizer with respect to 100 parts by mass of polyvinyl butyral. ..

(1)脱気性の評価
得られた表面に凹凸を有する合わせガラス用中間膜を用いて、以下に示すように、減圧脱気法で予備圧着を行い、次いで本圧着を行って、合わせガラスを作製した。
(1) Evaluation of degassing property Using the obtained interlayer film for laminated glass having irregularities on the surface, preliminary crimping is performed by the vacuum degassing method as shown below, and then main crimping is performed to obtain the laminated glass. Made.

(減圧脱気法)
中間膜を二枚のクリアガラス板(縦30cm×横30cm×厚さ2.5mm)の間に挟み、はみ出た部分を切り取り、こうして得られた合わせガラス構成体(積層体)をゴムバッグ内に移し、ゴムバッグを吸引減圧機に接続し、加熱すると同時に−60kPa(絶対圧力16kPa)の減圧下で10分間保持し、合わせガラス構成体(積層体)の温度(予備圧着温度)が70℃となるように加熱した後、大気圧に戻して予備圧着を終了した。尚、上記予備圧着時の脱気開始温度は40℃、50℃及び60℃の3条件で行った。
(Decompression degassing method)
The interlayer film is sandwiched between two clear glass plates (length 30 cm x width 30 cm x thickness 2.5 mm), the protruding part is cut off, and the laminated glass structure (laminated body) thus obtained is placed in a rubber bag. Transfer, connect the rubber bag to a suction decompressor, heat it and hold it under reduced pressure of -60 kPa (absolute pressure 16 kPa) for 10 minutes, and the temperature (preliminary crimping temperature) of the laminated glass structure (laminate) is 70 ° C. After heating to the above, the pressure was returned to atmospheric pressure to complete the preliminary crimping. The degassing start temperature at the time of the preliminary crimping was performed under three conditions of 40 ° C, 50 ° C and 60 ° C.

(本圧着)
上記方法で予備圧着された合わせガラス構成体(積層体)をオートクレーブ中に入れ、温度140℃、圧力1300kPaの条件下で10分間保持した後、50℃まで温度を下げ大気圧に戻すことにより本圧着を終了して、合わせガラスを作製した。
(Main crimping)
The laminated glass structure (laminate) pre-crimped by the above method is placed in an autoclave, held for 10 minutes under the conditions of a temperature of 140 ° C. and a pressure of 1300 kPa, and then lowered to 50 ° C. and returned to atmospheric pressure. The crimping was completed to prepare a laminated glass.

(合わせガラスのベークテスト)
得られた合わせガラスを140℃のオーブン中で2時間加熱した。次いで、オーブンから取り出して3時間放冷した後、合わせガラスの外観を目視で観察した。各20枚についてガラス板と合わせガラス用中間膜との間に発泡(気泡)が生じた枚数を調べて、全ての条件下において発泡枚数が5枚以下であった場合を「○」と、発泡枚数が6枚以上であった場合を「×」と評価した。
(Bake test of laminated glass)
The obtained laminated glass was heated in an oven at 140 ° C. for 2 hours. Then, after taking it out of the oven and allowing it to cool for 3 hours, the appearance of the laminated glass was visually observed. For each of the 20 sheets, the number of foams (bubbles) generated between the glass plate and the interlayer film for laminated glass was examined, and when the number of foams was 5 or less under all conditions, the number of foams was marked with "○". When the number of sheets was 6 or more, it was evaluated as "x".

(2)光学歪みの評価
観測者から7m離れた地点に蛍光灯(パナソニック社製 FL32S.D)を置き、蛍光灯と観測者を結んだ直線上の観測者から40cm離れた地点に、得られた合わせガラスを水平面に対して20°になるように、傾けて設置した。合わせガラスを通して、蛍光灯が歪んで見えた場合を×、見えない場合を〇とした。
(2) Evaluation of optical distortion A fluorescent lamp (FL32SD manufactured by Panasonic Corporation) is placed at a point 7 m away from the observer, and it is obtained at a point 40 cm away from the observer on the straight line connecting the fluorescent lamp and the observer. The laminated glass was installed at an angle so as to be 20 ° with respect to the horizontal plane. The case where the fluorescent lamp looked distorted through the laminated glass was evaluated as x, and the case where it could not be seen was evaluated as 〇.

(3)多重像発生の評価
輝度の異なる2種類の光源1及び光源2を用いて、多重像の発生の有無を評価した。ここで光源1は、10Wシリカ電球(旭光電機社製、PS55 E 26 110V−10W、全光束70lm)であり、自動車、航空機、建築 物等の窓ガラスに入射し得る一般的な輝度の光源を想定したものである。また、光源2は、40Wシリカ電球(朝日電器社製、LW100V38W−W 、全光束440lm)であり、自動車、航空機、建築物等の窓ガラスに入射 し得る光の中でも特に高輝度の光源を想定したものである。JIS R 3212(2008)に準拠する方法により、得られた合わせガラスの多重像の発生の有無を評価した。その結果、光源1、光源2のいずれを用いたときにでも、単一像が観察されるか、又は、15分以内の2重像が発生した場合を「○○」と、光源2を用いたときには多重像が発生するものの、光源1を用いたときには、単一像が観察されるか、又は、15分以内の2重像が発生した場合を「○」と、光源1、光源2のいずれを用いたときにでも、3重像が発生した場合を「×」と評価した。
なお、実車取付角度は30°に設定し測定を行った。また、A層の表面に付与した刻線状の凹部と、水平方向とが成す角を5°となるように配置し、C層の表面に付与した刻線状の凹部と、水平方向とが成す角を−5°となるように配置した。
また、15分以内の2重像とは中間膜に起因する像ではなく、ガラスに起因する像であった。
(3) Evaluation of Multiple Image Generation The presence or absence of multiple image generation was evaluated using two types of light sources 1 and 2 having different brightness. Here, the light source 1 is a 10 W silica light bulb (manufactured by Asahi Kodenki Co., Ltd., PS55 E 26 110 V-10 W, total luminous flux 70 lm), and is a light source having a general brightness that can be incident on the window glass of an automobile, an aircraft, a building, or the like. This is what I expected. The light source 2 is a 40 W silica light bulb (manufactured by Asahi Electric Co., Ltd., LW100V38W-W, total luminous flux 440 lm), and is assumed to be a particularly bright light source among the light that can be incident on the window glass of automobiles, aircrafts, buildings, etc. It was done. The presence or absence of multiple images of the obtained laminated glass was evaluated by a method according to JIS R 3212 (2008). As a result, when a single image is observed or a double image is generated within 15 minutes regardless of whether the light source 1 or the light source 2 is used, the light source 2 is used as "○○". When multiple images are generated, when the light source 1 is used, a single image is observed, or when a double image is generated within 15 minutes, "○" is given to the light source 1 and the light source 2. Regardless of which one was used, the case where a triple image was generated was evaluated as "x".
The actual vehicle mounting angle was set to 30 ° for measurement. Further, the engraved concave portion provided on the surface of the A layer and the engraved concave portion provided on the surface of the C layer are arranged so that the angle formed by the horizontal direction is 5 °, and the engraved concave portion provided on the surface of the C layer and the horizontal direction are formed. The angle formed was arranged so as to be −5 °.
Further, the double image within 15 minutes was not an image caused by the interlayer film but an image caused by glass.

Figure 0006856713
Figure 0006856713

Figure 0006856713
Figure 0006856713

本発明によれば、2層以上の樹脂層が積層された合わせガラス用中間膜であって、合わせガラスの製造工程において優れた脱気性を有し、かつ、多重像の発生を防止できる合わせガラス用中間膜、及び、該合わせガラス用中間膜を含む合わせガラスを提供することができる。 According to the present invention, it is an interlayer film for laminated glass in which two or more resin layers are laminated, has excellent degassing property in the manufacturing process of laminated glass, and can prevent the generation of multiple images. An interlayer film for use and a laminated glass containing the interlayer film for laminated glass can be provided.

1 任意に選択した一の凹部
2 任意に選択した一の凹部に隣接する凹部
3 任意に選択した一の凹部に隣接する凹部
A 凹部1と凹部2との間隔
B 凹部1と凹部3との間隔
10 樹脂層
20 多数の凹部と多数の凸部とを有する表面を有する樹脂層
21 樹脂層20の多数の凹部と多数の凸部とを有する表面
22 樹脂層20の樹脂層10と接していた側の表面
30 樹脂層
1 Arbitrarily selected one recess 2 Adjacent to an arbitrarily selected one recess 3 Recess adjacent to an arbitrarily selected one recess A Spacing between recess 1 and recess B Spacing between recess 1 and recess 3 10 Resin layer 20 Resin layer having a surface having a large number of concave portions and a large number of convex portions 21 Surface having a large number of concave portions and a large number of convex portions of the resin layer 20 22 The side of the resin layer 20 in contact with the resin layer 10 Surface 30 resin layer

Claims (7)

2層以上の樹脂層が積層された合わせガラス用中間膜であって、
少なくとも一方の表面に、多数の凹部と多数の凸部とを有し、前記凹部は、底部が連続した溝形状を有し、隣接する前記凹部が平行して規則的に並列しており、
前記多数の凹部と多数の凸部とを有する表面は、JIS B−0601(1994)に準拠して測定される凹部の溝深さ(Rzg)が10〜40μmであり、かつ、
前記多数の凹部と多数の凸部とを有する表面を有する樹脂層を、該樹脂層が直接接する樹脂層から剥離した後に、剥離した多数の凹部と多数の凸部とを有する表面を有する樹脂層の前記直接接していた樹脂層側の表面をJIS B 0601(1994)に準拠して測定した十点平均粗さ(Rz)が2.7μm未満である
ことを特徴とする合わせガラス用中間膜。
An interlayer film for laminated glass in which two or more resin layers are laminated.
At least one surface has a large number of concave portions and a large number of convex portions, and the concave portions have a groove shape with a continuous bottom portion, and the adjacent concave portions are parallel and regularly arranged in parallel.
The surface having a large number of concave portions and a large number of convex portions has a groove depth (Rzg) of the concave portion measured in accordance with JIS B-0601 (1994) of 10 to 40 μm and has a groove depth (Rzg) of 10 to 40 μm.
After peeling the resin layer having a surface having a large number of concave portions and a large number of convex portions from the resin layer in which the resin layer is in direct contact, the resin layer having a surface having a large number of peeled concave portions and a large number of convex portions is peeled off. A laminated glass interlayer film having a ten-point average roughness (Rz) of less than 2.7 μm measured in accordance with JIS B 0601 (1994) on the surface of the resin layer side that was in direct contact with the above.
隣接する凹部が平行して等間隔に並列していることを特徴とする請求項1記載の合わせガラス用中間膜。 The interlayer film for laminated glass according to claim 1, wherein adjacent recesses are parallel and parallel at equal intervals. 樹脂層は、ポリビニルアセタールと可塑剤とを含有することを特徴とする請求項1又は2記載の合わせガラス用中間膜。 The interlayer film for laminated glass according to claim 1 or 2, wherein the resin layer contains polyvinyl acetal and a plasticizer. 少なくとも第1の樹脂層と第2の樹脂層とを有し、前記第1の樹脂層に含まれるポリビニルアセタールの水酸基量が、前記第2の樹脂層に含まれるポリビニルアセタールの水酸基量と異なることを特徴とする請求項3記載の合わせガラス用中間膜。 It has at least a first resin layer and a second resin layer, and the amount of hydroxyl groups of polyvinyl acetal contained in the first resin layer is different from the amount of hydroxyl groups of polyvinyl acetal contained in the second resin layer. 3. The interlayer film for laminated glass according to claim 3. 第1の樹脂層におけるポリビニルアセタール100質量部に対する可塑剤の含有量が、第2の樹脂層におけるポリビニルアセタール100質量部に対する可塑剤の含有量と異なることを特徴とする請求項3記載の合わせガラス用中間膜。 The laminated glass according to claim 3, wherein the content of the plasticizer with respect to 100 parts by mass of polyvinyl acetal in the first resin layer is different from the content of the plasticizer with respect to 100 parts by mass of polyvinyl acetal in the second resin layer. For interlayer film. 遮音層が2層の保護層の間に積層された合わせガラス用中間膜であって、
前記遮音層は、ポリビニルアセタール100質量部に対して可塑剤を45〜80質量部含有し、前記保護層は、ポリビニルアセタール100質量部に対して可塑剤を20〜45質量部含有し、
前記保護層の少なくとも一方の表面に、多数の凹部と多数の凸部とを有し、前記凹部は、底部が連続した溝形状を有し、隣接する前記凹部が平行して規則的に並列しており、
前記保護層の多数の凹部と多数の凸部とを有する表面は、JIS B−0601(1994)に準拠して測定される凹部の溝深さ(Rzg)が10〜40μmであり、かつ、
前記多数の凹部と多数の凸部とを有する表面を有する保護層を遮音層から剥離した後に、剥離した保護層の遮音層側の表面をJIS B 0601(1994)に準拠して測定した十点平均粗さ(Rz)が2.7μm未満である
ことを特徴とする合わせガラス用中間膜。
An interlayer film for laminated glass in which a sound insulation layer is laminated between two protective layers.
The sound insulation layer contains 45 to 80 parts by mass of a plasticizer with respect to 100 parts by mass of polyvinyl acetal, and the protective layer contains 20 to 45 parts by mass of a plasticizer with respect to 100 parts by mass of polyvinyl acetal.
The protective layer has a large number of concave portions and a large number of convex portions on at least one surface of the protective layer, and the concave portions have a groove shape with a continuous bottom portion, and the adjacent concave portions are regularly arranged in parallel. And
The surface of the protective layer having a large number of concave portions and a large number of convex portions has a groove depth (Rzg) of the concave portion measured in accordance with JIS B-0601 (1994) of 10 to 40 μm and has a groove depth (Rzg) of 10 to 40 μm.
After peeling the protective layer having a surface having a large number of concave portions and a large number of convex portions from the sound insulation layer, the surface of the peeled protective layer on the sound insulation layer side was measured in accordance with JIS B 0601 (1994). An interlayer film for laminated glass, characterized in that the average roughness (Rz) is less than 2.7 μm.
少なくとも2枚のガラス板の間に請求項1、2、3、4、5又は6記載の合わせガラス用中間膜が積層された積層体を、ガラス板と中間膜との間に残留する空気を脱気しながら予備圧着する工程と、前記予備圧着後の積層体を、加熱加圧して本圧着する工程を有することを特徴とする合わせガラスの製造方法。A laminated body in which the interlayer film for laminated glass according to claim 1, 2, 3, 4, 5 or 6 is laminated between at least two glass plates, and the air remaining between the glass plates and the interlayer film is degassed. A method for producing a laminated glass, which comprises a step of pre-crimping while pre-crimping, and a step of heating and pressurizing the laminated body after the pre-crimping to perform main crimping.
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